Title of Invention

METHOD FOR PREPARING TRIMETHYLOLPROPANE

Abstract The present invention relates to a method for preparing trimethylolpropane (TMP) comprising the steps of: 1) synthesizing trimethylolpropane by using n-butyl aldehyde, an aqueous solution of formaldehyde and an aqueous solution of alkali metal hydroxide through aldol condensation reaction and Cannizzaro reaction; 2) extracting trimethylolpropane from a resultant mixture of the step 1) by contacting the resultant mixture with an alcohol having 6 to 10 carbons; 3) removing alkali metal ion from a resultant extract of the step 2) by contacting the resultant extract with water; and 4) distilling the alkali metal ion-removed extract obtained from the step 3). According to the present invention, a separate formaldehyde recovery process can be omitted, the extraction efficiency of TMP can be maximized with using a relatively small amount of extraction solvent, the separation and recovery processes for extraction solvent can be simplified since a mixture of solvents is not used for TMP extraction, and the yield of TMP can be maximized while the amount of generated waste water can be minimized, thereby producing TMP economically with good efficiency.
Full Text

Description METHOD FOR PREPARING TRIMETHYLOLPROPANE
[1] TECHNICAL FIELD
[2]
[3] The present invention relates to a method for preparing trimethylol propane (TMP),
Specificaly. the present invention relates to a method for preparing trimethyHpropane comprising the steps of: synthesizing irimetbylolpropane from n-butyl aldehyde, an aqueous solution of formaiiehjde, and an aqueous sdution of alkali metal hydroxide through liUd condensation reaction and Cannuzaro reaction: extracting trimethy- propane from the resultant mixture by using an alcohol having 6 to 10 carbons, preferably an alcohol having 8 carbons, and more preferably 2-echylhexanoi; removing alkali metal inn from the resultant extract by using water; and distilling the aikaE meia! ion-removed extract. According to the present invention, TMP can be prepared and extracted in good efficiency, with reducing the use amounts of sot vent for extracting TMP and water for removing alkali metal ion, by separating the TMP extraction step and the alkaly metal ion-removal step.
[4]
[5] BACKGROUND ART
[6]
|7] Trimethyfcipropane widely used its starting materia! in various applications such as atkyd resin, saturated polyester, synthetic lubricant oil. potoirethane resin, plasiieizer and the like. Ac¬cording, there have been continuous researches for economical producing TMP Lhat is an industrially important source material.
18J TMP is synthesized from n-butyl tiiehyde. on-BAL}. form aldehyde, and alkali
metal hydroxide through alio! condensation leacrion and Cannu/aro read ion as represented by the flowing reaction schemes i and 2;
[9[10] Reaction Scheme 1; AUd condensation reaction
[11]
CH3CH2CH:CHO + 2HCHO -» CH3CH2C(CH2OH) 3CHO
[i?l Reaction Scheme 2 : Canni/./aio reaction

114}
CH3CH2C(CH2OH) 3CHO + HCHO + NaOH ■*
CH3CHzC(CH2OH) 3 + HCOONa
1'5]
116| USP 3,L83,274 discloses a process for producing TMP wherein an excess amount
of k>nru4jeh>de is used to increase the production vietl, and a concentration step is incorporated before the extraction step to reduce the amount of extraction solvent. However, the '274 process requires an additional process for recovering formalleh\de remaining after the reaction since formallehjde is excessively used to increase the production \tcii. Also, in the l274 process, a large amount of extraction solvent, about 7 times as much as the amount of raw material, is used to increase the TMP extraction efficiency from a mixture resulted from the sjnihesis reactions. Thus, the '274 process was disadvantageous in that the costs for facJttes to recover the solvent are increased. whereby the investment costs and operational costs are increased. Further, in the "274 process, when extracting TMP by using organic solvent from a mixture resulted from the reaction despite using excessive amounts of formaldehyde and water, the resultant organic extract of TMP contains a considerable amount of sodium formate. Thus, this process has a problem that discofrratfon of TMP may be caused when the organic extract of TMP was distiled under vacuum.
[17] Also, USP 3,956,306 discloses a method for separating TMP from a resultant
reaction mixture by using two extraction solvents. However, the '306 method requires additional two separation steps for recovering the two extraction solvents used in the extraction step after the extraction is completed. Further, the amount of alkali metals present in the finally purified TMP is too high by about 42 ppm.
| i SI Moreover, USP 4,594,461 discloses a method for synthesizing TMP by syn-
thesizing dimethyiibutanal as intermediate by using trialkjlamine catalyst, and hy-drogenating it by using Pb catalyst However, the '461 method requires high temperature and high pressure, and thus the costs for facilities satisfying the reaction conditions are high. Further, the >ieH is decreased when amine is used as cataK'sr over a tong period of time, and so periodic change of the catalyst is required to obtain an ap¬propriately stable yield, whereby the cost for such change is additional needed.
119) As described above, the conventional methods for producing TMP have used an
excessive amount of starting materia! to increase the reaction \ieU, or tried to use various extraction solvents or conditions to separate TMP from alkali mead salt

venerated durius ihe reaction. As a result, a considerable amount of TMP is bsi during Lhe extraction sic-p. and the scale of facilities for extraction and recovery cannot but be mcieaxcd due to lhe excessive use of extraction solvent, and thus the conventional methods have had limited commercial application. Further, in the conventional methods as described above, the amount uf alk:tli meld remaining in she resultant even after the alkali metal salt-removing step is as considerably high as 40 ppm or more, and the remaining alkali metd may cause decomposition of TMP by high temperature during a subsequent vacuum distlation step for purifying TMP to highly purified product, resulting in discoloration of the final product.
[201
[21] DISCLOSURE OF THE INVENTION
[22]
123 j The present invention is to solve the problems of the conventional methods a>
described above. Therefore, the object of ihe present invention is to provide a method for preparing purified TMP from the starting materials of n-butyl aUehjdc, an aqueous solution of formal1eh\de, and an aqueous solution of alkali metal hydroxide , in au effective and economical wav without usin& manv extraction solvents.
[24]
[2.5] According to the present invention, the method for preparing trimethyiipropane
comprises the steps of:
[26] 1) s\nthesi/ing trimethyUpropane by using n-buty! aldehyde, an aqueous solution
of formaUelnde and an aqueous solution of alkali metal Indroxide
[271 through aldol condensation reaction and Canni7./aro reaction:
[2K] 2 * extracting frimethylnlpropane from a resultant mixture of the step 1} by
contacting the resultant mixture with an alcohol having 6 to 10 carbons;
|20| V* removing alkali metal ion from a resultant extract of the step 2) by contacting the
resultant extract with water: and
[30} A ) distiting the a'ktiS meta* ion-removed extract obtained from the step .^).
mi
\32\ BRIEF DESCRIPTION OF DRAWINGS
133)
[34| Figure 1 represents a process diagram of an embodiment of apparatus and line con-
struction for executing the method for preparing TMP according to the present invention.
13.51

\?(y\ "* Svrobds shown in figure 1
|37j [ : Reactor
|3K| 2 : M ulli-siage extractor
J39| 3 : M ulti-siage washing device
[401 4 • D isolation cdumn for recovering sdvent
(41 ] 5 : D jstflarion cdumn for removing lower boiling point materid
|42| fi: D isolation column for removing higher boiling point material
[43j 10. II. 12. 13, 14, 15, 16. 17, IK. 19. 20. 2L 22. 23. 24, 25 and 26 : Line
144 J
145] BEST MODE FOR CARRYING OUT THE INVENTION
146]
{47J Each sub-step of the method for preparing TMP according to the present invention
is described specifically below.
[48]
!49j In the step 1) of the method according TO the present invention, TMP is synthesized
by using n-butyl aldehyde, an aqueous solution of formdlehyde and an aqueous sdution of alkaE metal hydroxide through lild condensation reaction and Cannizzaro reaction. In this step, the n-butvi aldehyde, the aqueous solution of formaUchyJc, and the aqueous sdution of alkaE metal hydroxide may be fed into a reactor in which con¬densation reaction and Cannizzaro reaction are conducted, at the same time, or some of them may be fed earlier OnJy, to improve tbe reaction efficiency, it is preferable to feed the aqueous solution of formaUehjde earlier than the n-butyl aldehyde and the aqueous solution of alkali metal hydroxide, into the reactor. Also, in terms of reaction efficiency, it is preferable to feed the n-butyi uLlehyde into the reactor for 70 to 120 minutes, and the aqueous sdution of Jkali metal hydroxide for 70 to 90 minutes.
|50] Also, in the step 1), it is preferable to use * to 5 motes of formaldehyde in the
formaldehyde aqueous solution to one mole of n-butyl aldehyde. Also, the symhesis or TMP !S preferably conducted at 20 to 70 *C for90 to ISO minutes. In the present invention, if the formaldehyde amount and the synthesis temperature and time in ihe step 1) are within ihe above preferred ranges, the synthesis of TMP can be optimized. and so no additional process for recovering formaldehyde is needed,
(511 Further, in the step I *, lithium hydroxide, sodium hydroxide, potassium hydroxide
or mixtures thereof mav be used as the alkali metal hydroxide.
» «*
1521 in the step I i of the method according to the present invention, after completing
add condensation reaction and Cannizzaro reaction in which n-butyl akdehyde. an

aqueous solution of formalieh\de and. an aqueous solution of a]k;*!r metal hjdroxide are used as reactauLs, an organic add such as formic acid is added to a resultant mixture to neutralize un-reacted reaetants and control the pH. within 5 to 7. After completing the neutralization, water in the resultant mixture is removed, for example, by vacuum d isolation. In the vacuum distillation, the amount of water removed therefrom is preferabfr 65 to 75 parts by weight per 1 00 parts by weight of water present in the resultant mixture fed for the vacuum distSation. in terms of efficiency in the subsequent extraction and alkali \x\eti removal steps. The above svnthesis reactions, each sub-step for neutralization and concentration, may be conducted se¬quential** in a single reactor or each separate reactor step by step.
1531
1541 In the step 2) of the method according to the present invention. TMP is extracted
from a resultant mixture of the step I) by using an alcohol having 6 10 10 carbons, preferahfy an alcohol having 8 carbons, and more preferabV 2-ethyihexand, as extraction solvent, if the extraction solvent is an alcohd having less than 6 carbons or more than 10 carbons, the extraction efficiency is decreased. Further, in die step 2), the amount of the alcohol having 6 to 10 carbons is preferably 1 to 2 times the weight of the resultant mixture of the step 1), and the extraction of TMP is preferabV conducted at 30 to SO °C for 30 to 90 minutes. In the step 2) of the present invention, if the amount of ;icohd having 6 to 10 carbons and the extraction temperature and time are within the above preferred ranges, the extraction of TMP is optimized, and so sub¬stantial 100 % of TMP present in the resultant mixture of the step 1) can be recovered as organic layer, i.e. alcohol layer used as extraction solvent.
\55] The extraction device used in the step 2) is not particularly limited, and thus a
muiti-stace extractor such as Scheibel-tvpe of multi-stage extractor conventional used for extraction of a specific target materia! usinjr an extraction solvent in this ileU may be u>ed.
[56]
|571 In the step 3) of the method according to the present invention, alkali metal ion is
removed from a resultant extract of the step 2) by using water. For the step 3) of the present invention, it is preferable to use ddoni/ed water, and the amount of used water is preferably 5 to 20 parts by weight to KM) parts by weight of the resultant extract of the step 2). Also, the removal of alkali metal ion is preferably conducted at 30 to K0 yC for 30 to 90 minutes, in the present invention, if the amount of used water and the temperature and time t'o\- the removal in the step 3) are within the above preferred

ranges, the removal of alkoE rncial ion is optimized, and So the ion-removed extract
obtained from the step ?) can contain alkali metal ions in 40 ppm or less, preferably 35
ppm or less, and more preferably 30 ppm or less.
[581
[59] The device used in the step 3) is not particularly limited, and thus a multi-stage
washing device such as Scheibel-type of multi-stage washing device conventional.-
used in this fieil may be used.
jfiOj According to a preferred embodiment of the present invention, the loss of TMP in
the step 3) can be. reduced by recycling the water used in the step 3) into a reactor
conducting the step I u and thus the TMP yieii of the overal process can be increased.
1611
1621 In the step 4} of the method according to the present invention, purified TMP is
produced by disriEng the alkafi metal ion-removed extract obtained from the step 3). According to a preferred embodiment of the present invention, in the step 4). the alcohol havins 6 to JO carbons which has been used as extraction sdvent in the previous step 2} is distied first and recovered or recycled into the step 2), and then fower boiling point material and higher boiling point material are removed sequential by distflation to produce TMP with high purity. For the distflation of alcohol used as extraction solvent, a conventional multi-stage distflation apparatus such as 15-stage OUershaw distillation apparatus may be used, and the condition for the distflation of alcohol may be varied depending on the types of alcohd and apparatus. Preferable conditions for the distillation may be a distflation cdumn pressure of 200 to 250 robar. a temperature of 130 to 1&0 °C , and a reflux ratio of 0.1 to 1. After the dis¬tflation of alcohol used as extraction solvent, lower boiling point material and higher boiling point material are removed sequential^ by using a conventional vacuum di.s-fflurinn apparatus. Here, the "lower boiling point material" refers to a materia which has a lower boiling point than TMP among organic compounds excluding TMP. water. alcohol as extraction solvent, and :^ikrdi metal salt of formic acid, and the 'higher boiling poim material' refers to a material which has a higher boiling point than TMP among organic compounds excluding TMP, water, alcohol as extraction solvent, and aikiii metal salt of formic acid. The conditions for distflation of lower boiling point material and higher boiBng point material may be varied depending on the types of distiled material and distillation apparatus.
1631
|64) With reference u\ Figure 1. the present invention is described more specificaly

hek.m.
|65j
[66 j figure I i.s a process diagram for an embodiment of apparatus and tine construction
for executing the method for preparing TMP according to the present invention.
|67| In Figure 1, a formaldehyde aqueous solution, n-buty] adehule (n-BALh and an
aqueous solution of a]kali metaJ hjdroxide such as NaOH are fed into the* reactor (1) through the three lines (10. ] 1 and 12), respectively, in a preferred embodiment, a certain amount of the forrnafciehvde aqueous solution is fed first into the reactor (i i, and then the n-hutyj aUeh}de and the aqueous solution of alkali meld hvdroxide are fed into the reactor c 1) continuous!)' for a certain period of time. Here, preferably, the amounts of formrilehuJe and alkali.metal hjdroxide aie 3 to 5 moles and 1 to ! .5 moles, respective^, to one mole of n-BAL- After completing the feeding, the reactions are conducted ax 20 to 70 CC for90 to ISO minutes to synthesize TMP. After completing the reactions, a certain amount of formic acid is fed into the reactor (1) through the fine (13) to neutraEze the resultant mixture to a level of pH 5 to 7. After completing the neutralization, the resultant mixture is distied under vacuum to remove excessive water present therein through the line (15). At this time, if 65 to 75 parts by weight of water to 100 parts by weight of water present in the resultant mixture fed for the vacuum distillation is removed, a concentrated resultant mixture containing 40 to 50 weigh* % of TMP is obtained.
168]
[69] Next, the concentrated resultant mixture obtained above is fed continuous^ into
the multi-stage extractor (2) for extracting TMP through the Kne (16). Meanwhile, as
extraction solvent, an alcohol having 6 to 10 carbons, preferable an alcohol having S
carbons, and more preferably' 2-ethyLhexaiioL is fed into through the line (21) by 1 to 2
limes the weight of the concentrated resultant mixture, and then TMP is extracted at 30
to KO CC for 30 to 90 minutes. The resultant extract containing TMP is discharged from
the multi-stage extractor (2 i through the line 117).
|70f Then, the TMP-eontaining resultant extract obtained above is fed continuous^ into
the multi-stage washing device (3) through the line (17) while water for washing is fed into through the line (19* by 5 to 20 parts by weight of water to 100 parts by weight of the TMP-eontaining resultant extract. And. the resultant extract is washed at 30 to SO CC for 30 to 90 minutes. The water used in the washing is discharged from the multi¬stage wa.shing device (?) through the tine ( 14». thereby removing alkali metal salt contained in the TMP-eontaining extract. The water discharged through the line i. 3 4 (is

recycled into the reactor (I) 10 minimize the bss of TMP,
|7| j Next, the TMP-containing extract obtained by washing ;md removing alkali metal
ion is fed into the disinflation column (4) for recovering solvent through the line (20). In the distillation cdumn (4i the ;ieohd used as extraction sdvent is distifled and recovered, and the recovered alcohd is recycled into the multi-stage extractor (2) through the line (2 ] > to minimize bss of the extraction solvent. Then, the TMP-containine resultant extract which is obtained bv the distDation oi the extraction sdvent is fed sequential into the distillation columns p) and ifo which use vacuum distilation conventional known in the art, thereby removing sequentially bwer boiBng point material and higher boiling point material present in the extract together with TMP. Iin%. TMP product with high purity is discharged through the line (25),
and other residues arc discharged through the line (26).
i -> -J I
! '-!
173] As described above, in the present invention, aseparate formaUehyde recovery
process may be omitted by optimizing the use amount of formaldehyde and the reaction conditions for TMP synthesis. Also, the present invention can maximize the TMP extraction efficiency by selecting optimum extraction sdvent and extraction conditions, with using relative^ a small amount of extraction sdvent. Further, in the present invention, the separation and recovery processes for extraction sdvent can be simplified since a mixture of solvents is not used for TMP extraction. Also, the yield of TMP can be maximized, and the amount of waste water generated therein can be mijiimued. bv recycling I he water used in the washing into reactors,
[74]
[75J The present invention can be more specific^ explained by the felling
examples. However, it shouli be understood that the present invention is not Eimited by these examples in any manner.
|*76|
[77] Example 1
[7K]
179) 1) Synthesis of TMP and concentration of the resultant mixture
ISO!
[SI j 390.6 g (A.X md) of forrnatiehule and 719.2 g of deionized water were fed in\o a
2 L reactor. Then, into the reactor, 108.2g
reactor temperature at the rime of feeding the reactants was maintained at 45 ::C . After completing the feeding, the reactor temperature was elevated to 50 5C , a«d the synthesis was further conducted for 30 minutes. After the further -synthesis for 30 minutes, the resultant mixture contained 182.2 g (1.4 mol) of TMP, which Ls an amount corresponding to 13.5 parts by weight to 100 parts by weight of the resultant mixture.
|K2| The resultant mixture was fed with 7.7 g of formic acid for neutralization, and
distfled under vacuum. Then, water was removed through the top of the reactor lo obtain 3(tt,X g of concentrated resultant mixture. The resultant mixture and the con¬centrated resultant mixture were analyzed by using Gas Chromatography. The analysis results are shown in Table 1 bebw.
f83j

185] 2) Extraction of TMP
186]
[87 j The concentrated resultant rtuxture obtained from the step I} was fed into the top
oi a 7 L Scheibel-type multi-stage extractor at the rare of 40 g/min while 2-erhylhexanol as extraction solvent was fed continuously- into the bottom of the multi¬stage extractor at the rale oi 60 g/min. thereby extracting TMP. The extraction temperature was 60 SC . As a resultant extract, TMP-comuiniug --eihylhexam.j Nijution was obtained through the lop of the multi-stage extractor at the rate of K3.3 g/ min. There was no bss of TMP during the extraction (J 00 % of extraction efficiency). The analysis result io the resultant extract ate shown in Table 2 below,
I SRI
18? I 3) VVasliing of TMP for removing alkali metal ion
|911 The TMP- containing 2-ethylhexanol solution obtained from the step 2) was

cuSected and fed ijno the bottom of a 7 L Sehetbel-type multi-stage washing device at the rate of ] 00 g/inin white deionized water for washing was fed continuously into the ton of the muhi-stu&e washing device ai the rate of 8 g/miru therefav washing the TMP-containing 2-ethylhexanot solution to remove sodium ion present therein. The washing temperature was 60 °C . As a washed resultant extract, TMP- containing 2-eih}1hexanol stiuiion was; obtained through the top of the multi-stage washing device at the rale of 105.5 g/min. The content of sodium ion in the washed resultant extract was measured as 28 ppm by using an ion meter analyzer. The anaksis results to the washed resultant extract are show n in TabJe 2 hebw, 192]
193]
\94] 4) Instillation and recovery of extraction solvent and purification
of TMP
195]
[96J The washed resultant extract obtained from the step 3) was fed continuously* into a
suppK' end at the middle of a 15-stage OUershaw Uistlarion apparatus at the rale of 14.8 g/min to recover 2-ethyihexand used as extraction solvent. The disrilation conditions were the pressure of 200 rnbar. the temperature of 130 :C . and the reflux ratio of 0.5. A top effluent containing 99.5 weight '# of 2-ethylhexanci was recovered through the top of the distSation apparatus at the rate of 12.3 g/niin. and as a .sdvem-removed product, a bottom effluent containing M.S weight rA. of TMP was obtained through the bottom of the distillation apparatus.
[97] Then, from the solvent-removed product, bwer boiling point material was
removed by using a 15-stage Oliershaw distillation apparatus, thereby obtaining a bwer boffing point material-removed product. The conditions for removing bwer buffing point materia? was the piessure of 200 rnbar, the temperature of 131 CC , and

the reflux ratio of 2.0.
|9KJ Then, from the lower boiling poiai material-removed product higher bailing point
ma tend was removed by using a5-.stage OUershaw disfilation apparatus, thereby obtaining a final product of purified TMP (99.5 weight ck of TMP). The conditions for removing higher boning point material were the pressure of 5 mbar. the temperature of 223 DC , and the reflux ratio of 2.0. During the purification of TMP, discoloration of TMP was not observed. The analysis results to the solvent-removed product, die bwer buffing point mare rial-removed product and the final product of purified TMP are shown in Table 3 be-bw.

(100) Example 2
[101]
1102j . Purified TMP wax prepared according to the same method as Example 1, except
that 2-ethyihexanol was fed at the rale of 80 g/min in the .step 2), and detoni/ed water
was fed at the rate of 10 g/min in the step 3). There was no bss of TMP during the
extraction \ 100 -.t- of extraction efficiency;., and the content of sodium ion in the
washed resuliam extract was measured as 17 ppm.
[1031
fliMj Example 3
1105]
flOnl Purified TMP was prepared according to the same method as Hxample I, except
that 108.2 g (1,5 mol) of n-bun1atieli\de tn-B AD arid 138 g of 48 c/r aqueous solution of sodium hydroxide (1.7 md of sodium h\droxide) were ted continuously for 105 minutes and 90 minutes, respective^, in the step 1). The resultant mixture of the TMP synthesis contained t H1.7 o (1.4 mol) of TMP. which is an amount corresponding to

13.4 pans by weight to J 00 parts by weight of the resultant mixture. There was no Kss of TMP during the extraction (100% of extraction efficiency), and the content of sodium ion in the washed resultant extract was measured as 31 pprn.
fin/|
13 OK J Comparative Example 1
I109J
(1 10] In this Comparative Example, the extraction and washing of TMP were carried out
simultaneous^7 as follows.
[Ml| The concentrated resultant mixture obtained from the step 1 > of ExampJe I was fed
into the top of a 7 L Scheibel-iype multi-stage extractor at the rate of 40 g/min while 2-ethyihexano! as extraction sdvenl was fed continuously into the bottom of the multi¬stage extractor at the rate of 60 t*/min. And, deionixed water for washing was fed into the top of the multi-stage extractor at tie rate of 3.2 g/mint thereby extracting and washing TMP simultaneous^ in a single step. At that time, the extractor's temperature was 60 :C . As a resultant extract. TMP-containing 2-ethylhexanof solution was obtained through the top of the multi-stage extractor at the rate of 92.1 g/min. The extraction efficiency of TMP was as bw as 97,4 %r and the content of sodium ion in the washed resultant extract was measured as high as 4530 pprn.
[1121
[113] Comparative Example 2
[1U1
11151 in ibis Comparative Example, arayl alcohol having 5 carbons was used as
extraction solvent as falows.
11161 The concentrated resultant mixture obtained from the step I) of Example 1 was fed
into the top of a 7 L Scheibel-rype multi-stage extractor at the rate of 40 g/min white amy! alcohol as extraction solvent was fed continuousK' into the bonom of the multi¬stage extractor at the rate of SO g/min, thereby extracting TMP. The extraction temperature was 60 C . As a resultant extract, TMP-conlaining amy] alcohol sciution was obtained through the iap of the multi-stage extractor ai the rate of 94 g/min, Tlie extraction efficiency of TM P was as bw as 82 %.
IJ17J Then, the TMP-conraining amyl alcohd solution was collected ajid fed into the
bottom of a 7 L Scheibel-type multi-stage washing device at the rate of 80 g/min while deionixed water for washing was feu continuously' into the top of the multi-stage washing device al the rate of 44 g/min, thereby washing the TMP-containing amy] alcohol solution to remove sodium ion present therein. The washing temperature was

60oC As a washed resultant extract, TMP-containing aryl alcohol solution was obtained through the top of the multi-stage washing device at the rale of 68 g/min. The content of sodium ion in the washed resultant extract was measured as high as 5()i) ppm.
|118]
[119] INDUSTRIAL APPLICABILm7
[121 ] As described above, according to the present invention, a separate formalkhyde
recovery process may be omitted: the efficiency of TNI P extraction can be maximized with using a relatively' .smal amount of extraction solvent: the separation and recovery processes for extraction solvent can be simplified since a mixture of solvents is not used for TMP extinction; and the yield of TMP can be maximized while the amount of generated waste water can be minimized, thereby producing TMP economic* in good efficiency.

Documents:

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Patent Number 246102
Indian Patent Application Number 3003/CHENP/2007
PG Journal Number 07/2011
Publication Date 18-Feb-2011
Grant Date 14-Feb-2011
Date of Filing 05-Jul-2007
Name of Patentee LG CHEM, LTD
Applicant Address 20, YOIDO-DONG YOUNGDUNGPO-KU SEOUL 150-721
Inventors:
# Inventor's Name Inventor's Address
1 CHOE, JAE, HOON EXPO APT #401-704 JEONMIN-DONG YUSEONG-GU DAEJEON 305-762
2 REW, DAE, SUN SEJONG APT #109-302 JEONMIN-DONG YUSEONG-GU DAEJEON 305-728
3 EOM, SUNG, SHIK LG STAFF APT #5-204 DORYONG-DONG YUSEONG-GU DAEJEON 305-340
4 KO, DONG, HYUN PROFESSOR APT #11-301 GAJEONG-DONG YUSEONG-GU DAEJEON 305-350
5 MOON, JI, JOONG EXPO APT #106-201 JEONMIN-DONG YUSEONG-GU DAEJEON 305-761
PCT International Classification Number C07C 31/22
PCT International Application Number PCT/KR06/01233
PCT International Filing date 2006-04-04
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 10-2006-0021185 2006-03-07 Republic of Korea