CN100447120C - Process of refining trimethylolpropane - Google Patents

Process of refining trimethylolpropane Download PDF

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CN100447120C
CN100447120C CNB200610015698XA CN200610015698A CN100447120C CN 100447120 C CN100447120 C CN 100447120C CN B200610015698X A CNB200610015698X A CN B200610015698XA CN 200610015698 A CN200610015698 A CN 200610015698A CN 100447120 C CN100447120 C CN 100447120C
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tmp
trimethylolpropane
tower
solvent
processing method
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CN1919815A (en
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蓝仁水
黄贵明
郑铁江
余锦河
孙太喜
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Jiangsu Baichuan hi tech new material Co., Ltd
New Tianjin T & D Co ltd
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天津市新天进科技开发有限公司
无锡百川化工股份有限公司
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Abstract

The invention discloses a manufacturing method of trihydroxy methyl propane, which comprises the following steps: catalyzing aldehyde alcohol to condense in the inorganic alkaline through butyladehyde and formaldehyde; proceeding cross Connizzaro reaction to obtain TMP solution; adopting multi-grade evaporating condensing, counter current extracting counter current washing desalting and vacuum double-effect integrating to recycle solvent; flashing; distilling in the high vacuum; recycling TMP.

Description

The processing method of refining trimethylolpropane
Technical field
The invention provides a kind of processing method of refining trimethylolpropane, by butyraldehyde-n and formaldehyde in mineral alkali (oxyhydroxide of sodium, calcium, potassium and lithium) catalysis aldol condensation, and further intersect TriMethylolPropane(TMP) (hereinafter to be referred as the TMP) solution that Connizzaro (Connizzaro) reaction obtains, adopt that multistage evaporation concentrates, operations such as multi-stage counter current extraction and multi-stage countercurrent washing desalination, the integrated solvent recuperation of vacuum economic benefits and social benefits heat, flash distillation are taken off heavily, high vacuum rectification and TMP recoverys, can obtain stay-in-grade high purity at an easy rate and hang down colourity TriMethylolPropane(TMP) product.
Background technology
TriMethylolPropane(TMP) (Trimethylolpropane is called for short TMP) has another name called 2-ethyl-2-methylol-1, and ammediol (2-ethyl-2-(hydroxymethyl)-1,3-Propanediol), structural formula: CH 3CH 2C (CH 2OH) 3Normal temperature is white solid down, and boiling point is 295 ℃ under the normal pressure, 58~59 ℃ of fusing points, relative density 1.1758 (20 ℃).Be soluble in acetone, dissolve in tetracol phenixin, chloroform, the ether; Be insoluble to aliphatic and aromatic hydrocarbons.Stronger water absorbability is arranged.Containing three methylols on the α position of molecule, is a kind of trivalent alcohol of new penta structure.Have the resin of raising soundness, erosion resistance, stopping property; For hydrolysis, pyrolysis and oxidation tool satisfactory stability; Three hydroxyls have excellent performances such as equivalent responses.TMP has important industrial application value, can be used for the raw material of cold coating, urethane foam, polyether glycol, softening agent, lubricating oil, tensio-active agent, stablizer etc.
TMP is aldol reaction in the presence of mineral alkali (oxyhydroxide of sodium, calcium, potassium and lithium) catalyzer by butyraldehyde-n and formaldehyde, and condensation reaction products and formaldehyde further intersect Connizzaro (Connizzaro) and reacts and obtain TMP solution in the presence of basic catalyst.Use the two-step approach reaction formula of NaOH as follows:
The first step, aldol reaction:
Second step, cross Connizzaro reaction:
Mainly contain water, TMP, sodium formiate and a small amount of light constituent and heavy constituent impurity in the TMP solution by above-mentioned prepared in reaction.
Chinese patent 93100141.2 discloses a kind of TMP process for purification.With above-mentioned TMP solution through normal pressure concentrate, operation such as vacuum concentration, crystallization, centrifugation, mother liquid evaporation are refining, obtain the TMP product.Because water is all removed the operation energy consumption height in the reaction product by evaporation.In the treating process, salinity is only removed in Crystallization Separation, and more salinity enters the TMP Distallation systm, can cause when refining that TMP partly decomposes, and causes product purity, colourity relatively poor, and product yield is lower.
Chinese patent CN 98810172.6 discloses a kind of TMP process for purification, and its main path is a characteristic of utilizing the TMP fusing point higher.Allow solution be cooled to 20~50 ℃ of following phase-splittings at a lower temperature, separate purification TMP from washing or organic phase respectively then.Thisly descended the phase-splitting operation extensive operate continuously to be existed the risk of certain occluding device being lower than the TMP fusing point.Adopt this method to have salinity and the isolating problem of TMP equally from the refining TMP of water.
Chinese patent CN 99126564.5 discloses a kind of TMP process for purification, with above-mentioned TMP solution through the acid effect, make sodium formiate (HCOONa) inactivation that reaction generates after, heating removes high boiling point composition and inorganic salt, and thermal treatment under acidic conditions then obtains the TMP product by distillation again.Thisly when containing a large amount of high boiling point compositions and inorganic salt, just heat-treat, distillatory technology, be easy to cause that TMP partly decomposes, cause product purity, colourity relatively poor, product yield is lower.
Chinese patent CN 02159801.0 provides a kind of TMP process for purification, adopt the method for multistage distillation to remove moisture content and inorganic salt above-mentioned TMP solution, inter-stage adopts the differential pressure power-save operation, in above-mentioned multistage distillation process by filter, centrifugal or sedimentation separates residue with decantation.Distillation at last obtains the TMP product.This process for purification is close with the disclosed processing method of Chinese patent CN93100141.2, all is to dewater by the distillatory method.Concentrated energy consumption is very high, and because the existence of salinity, the TMP product yield is lower, purity and look number be cannot say for sure to demonstrate,prove.The advantage of Chinese patent CN 02159801.0 is that it has proposed multistage operations, the energy-conservation technology of inter-stage in dehydration, concentration process.Also mentioned among the Chinese patent CN 02159801.0 and adopt solvent extraction earlier in dehydration, concentration process, redistillation removes the operational path of solvent, and distillation obtains the TMP product then.Compare with aforementioned publication technology, this patent exists also that salinity removes halfway defective before the rectifying of TMP product, causes that the TMP product yield is lower, purity and look number cannot say for sure to demonstrate,prove.
Chinese patent 00818004.0 discloses a kind of TMP process for purification, and it is at adopting tertiary amine (being generally trialkylamine) to replace mineral alkali to carry out above-mentioned Connizzaro (Connizzaro) reaction.TMP solution refining process is the sepn process of materials such as water, trialkylamine (or formic acid trialkyl ammonium), TMP.And as said in the Chinese patent 00818004.0 " different methods of preparation TriMethylolPropane(TMP) requires different aftertreatments ", the mineral alkali catalysis process that adopts Chinese patent 00818004.0 to provide, " being reflected at 2; the 2-dihydroxymethyl butyraldehyde stage stops; this compound is converted into TriMethylolPropane(TMP) by hydrogenation then " of butyraldehyde and formaldehyde, be that the processing method that Chinese patent 00818004.0 provides must utilize the hydrogenation measure to obtain the TriMethylolPropane(TMP) product, and then carry out subsequent product and separate and purge process.Therefore, Chinese patent 00818004.0 is different fully with the TMP solution refining process that the present invention relates to, so document as a comparison not.
Chinese patent 02824171.1 discloses a kind of TMP process for purification, and its separated reactant is " react to reach in the presence of the tertiary amine of catalytic amount by butyraldehyde-n and formaldehyde and obtain with back end hydrogenation " mixture.Different fully with the reactant with mineral alkali catalysis acquisition provided by the invention.Therefore with Chinese patent 00818004.0 similarly, document as a comparison.Though, mention the method that it provides in the Chinese patent 02824171.1 and " both be suitable for aftertreatment by the Connizzaro method; i.e. the reaction mixture that in the presence of the alkali of stoichiometric quantity, obtains; be suitable for aftertreatment again and pass through method of hydrotreating; promptly in the presence of the tertiary amine of catalytic amount and " with the reaction mixture of back end hydrogenation acquisition, but, press the mineral alkali Catalytic processes, Chinese patent 02824171.1 just with obviously lacked lights removal, dehydration, operations such as salinity removes, and step dehydration and light constituent process energy consumption are very high, and the existence of salinity can cause the TMP product yield, problems such as purity and colourity are not good.
Summary of the invention
The processing method that the purpose of this invention is to provide a kind of refining trimethylolpropane, by butyraldehyde-n and formaldehyde at mineral alkali (sodium, calcium, the oxyhydroxide of potassium and lithium) catalysis aldol condensation, and further intersect TriMethylolPropane(TMP) (hereinafter to be referred as the TMP) solution that Connizzaro (Connizzaro) reaction obtains, the present invention adopts multistage evaporation to concentrate, multi-stage counter current extraction and multi-stage countercurrent washing desalination, the integrated solvent recuperation of vacuum economic benefits and social benefits heat, flash distillation is taken off heavily, operations such as high vacuum rectification and TMP recovery can obtain the low colourity TriMethylolPropane(TMP) product of stay-in-grade high purity at an easy rate.
The processing method of refining trimethylolpropane provided by the invention is in mineral alkali (oxyhydroxide of sodium, calcium, potassium and lithium) catalysis aldol condensation by butyraldehyde-n and formaldehyde, and further intersect Connizzaro (Connizzaro) reaction and obtain TriMethylolPropane(TMP) solution, the step of this processing method is that described TriMethylolPropane(TMP) solution is taken off steps such as weight, high vacuum rectification and recovery through concentrated, desalination, solvent recuperation, flash distillation;
1) described concentrate is to adopt single vaporization or multistage evaporation process to finish concentrating of TriMethylolPropane(TMP) solution, removes the most of moisture content in the solution, and formaldehyde, methyl alcohol light constituent;
2) described desalination is to adopt the organic solvent multi-stage counter current extraction, removes moisture content and salinity contained in the thick TriMethylolPropane(TMP) solution, and water is as extraction agent again, and the further desalination of TriMethylolPropane(TMP) solution concentration liquid is finished in washing through multi-stage countercurrent;
The miscible or only slight miscible above-mentioned concentration process of organic solvent extraction does not obtain TMP solution with water in employing, and TMP enters in the organic phase, and water and part salinity are at aqueous phase.Dehydration and most of desalination of the reaction product aqueous solution have been finished.Adopt multistage washing desalinating process then, washing further removes the salinity in the organic phase by the organic phase that aforesaid operations obtains.
3) described solvent recuperation is the purpose that the two tower differential pressures operation of solvent pairs recovery tower in the employing system reaches the integrated operation of economic benefits and social benefits heat, realizes solvent recuperation.
4) to take off heavily be the vaporization that utilizes heat-exchanger rig to finish to remove the thick TriMethylolPropane(TMP) product behind the solvent in described flash distillation, liquid phase is discharged remaining salinity and part heavy constituent, thick TriMethylolPropane(TMP) gas phase enters follow-up TriMethylolPropane(TMP) rectifying tower with liquid form after demist, condensation.
5) described high vacuum rectification is to utilize rectifying tower to operate under high vacuum, adopts the partitioned column structure, and thick TriMethylolPropane(TMP) enters dividing plate one side, the removed overhead light constituent, and the tower still is discharged heavy constituent, by tower middle part, dividing plate opposite side extraction TriMethylolPropane(TMP) product.
6) described recycling step is to utilize rectifying tower to handle TriMethylolPropane(TMP) rectifying tower cat head and tower still material respectively, reclaims wherein contained TriMethylolPropane(TMP).
Described organic solvent is the alcohol organic solvent that contains 5~9 carbon atoms, and described organic solvent is the independent a kind of or mixture of above-mentioned multiple solvent.Preferred 2-Ethylhexyl Alcohol, enanthol or hexalin equal solvent.
The condition of described organic solvent extraction operating process is: 0.05~1.0Mpa, 40~100 ℃; And preferred 0.1~0.5Mpa, 50~80 ℃.
The condition of described multi-stage countercurrent washing operating process is: 0.05~1.0Mpa, 30~90 ℃; And preferred 0.1~0.5Mpa, 40~70 ℃.
Described TriMethylolPropane(TMP) rectifying tower adopts the structured packing tower structure, adopts plate ripple arranged packing or screen waviness structured packing, general preferred screen waviness structured packing.
Described TriMethylolPropane(TMP) rectifying tower adopts the conventional rectification tower structure, extracts the TriMethylolPropane(TMP) product out by a certain position side line more than the charging.
Described TriMethylolPropane(TMP) is recovered as the optional process that improves the TriMethylolPropane(TMP) product yield, the recovery tower of TriMethylolPropane(TMP) rectifying tower cat head and tower still material is set as required simultaneously, a certain recovery tower in them perhaps only is set, or recovery tower is not set.
Described TriMethylolPropane(TMP) rectifying tower is liquid phase feeding or adopts gas-phase feed.
Described solvent recovery step adopts the integrated operational condition of double tower heat to be: solvent recovery tower A working pressure is 0.05~0.3Mpa, solvent recovery tower B working pressure is 0.001~0.05Mpa, and the material steam of solvent recovery tower A cat head is used for the material of a certain position of B charging of heated solvent recovery tower or heated solvent recovery tower B middle part.
It heavily is to operate under 0.0002~0.008Mpa condition that described flash distillation is taken off; The TriMethylolPropane(TMP) rectifying tower is to operate under 0.0003~0.008Mpa condition; Light constituent TriMethylolPropane(TMP) recovery tower is to operate under 0.001~0.05Mpa condition; Heavy constituent TriMethylolPropane(TMP) recovery tower is to operate under 0.0001~0.008Mpa condition.
Operations such as the present invention adopts that multistage evaporation concentrates, multi-stage counter current extraction and multi-stage countercurrent washing desalination, the integrated solvent recuperation of vacuum economic benefits and social benefits heat, flash distillation are taken off heavily, high vacuum rectification and TMP recovery, can obtain the low colourity TriMethylolPropane(TMP) product of stay-in-grade high purity at an easy rate, have the following advantages:
(1) adopts multi-stage solvent extraction and multistage washing desalinating process, removed the salinity among the TMP comparatively up hill and dale, can effectively avoid high-temperature heating process to cause the generation of TMP decomposition or other impurity to cause final TMP product purity and colourity variation.Can effectively improve the TMP product yield.
(2) the solvent recuperation operation has adopted the hot integrated technique of economic benefits and social benefits, adopts the operation of two tower differential pressures to reclaim solvent, and a solvent recovery tower overhead vapours is used for to another solvent recovery tower charging or a certain position heating of tower middle part, to reduce the operation energy consumption of solvent recuperation.
(3) the TMP rectification working process has adopted the gaseous condensate charging, technologies such as partitioned column high vacuum rectification.Before TMP rectifying, remove salinity and part heavy constituent once more, reduced TMP rectifying Tata still heavy constituent content effectively, reduce the generation of TMP decomposition and impurity.
(4) the structure strong guarantee of partitioned column the purity and the colourity of TMP product.Feed entrance point is in dividing plate one side, and the discharging position is positioned at the dividing plate right side, and non-volatility salinity and heavy constituent are split into the tower still in the charging left side in the charging; The charging opposite side is finished separating of light constituent and TMP, and final TMP product can obtain very high purity and very low colourity.
(5) the TMP recovery process is the additional part that further improves TMP overall product yield.
Description of drawings
Fig. 1 is a TMP purified process flow sheet provided by the invention.
Embodiment
A kind of TMP purified processing method provided by the invention, specific embodiments is described in detail as follows with reference to the technical process accompanying drawing:
Butyraldehyde-n and formaldehyde are in mineral alkali (oxyhydroxide of sodium, calcium, potassium and lithium) catalysis aldol condensation, and further intersect TriMethylolPropane(TMP) (hereinafter to be referred as the TMP) solution that Connizzaro (Connizzaro) reaction obtains, TMP crude product 1 through multiple-effect evaporation dehydration, after taking off light constituent enters extraction tower C401 top, organic solvent 2 counter current contact, multi-stage solvent extraction with the tower bottom charging, organic phase 4 is by the cat head discharging, and the tower still discharges brine waste 3.Organic phase 4 enters water wash column C402 bottom, and washing water 5 enter the C402 top, the two counter current contact, multistage washing, and the organic phase 9 after the washing is by the cat head discharging, and washing water 6 is by the discharging of tower still.For reducing the washing water yield, C402 can establish a circulation section in the bottom, and the part 8 of logistics 6 is returned C402 middle part, circulation cleaning, and another part 7 enters the C401 top.
Organic phase 9 after process extraction, the washing enters the bottom of solvent recovery tower A, and C601A tower still reboiler E602 adopts steam, thermal oil or the heating of other thermals source, and overhead vapours 10 enters hot integrated interchanger E601.C601A tower still high-temperature material 14 enters the E602 tube side after the step-down flash distillation, in logistics 10 heat exchange, the phlegma 11 of logistics 10 is divided into two strands, one material 12 is back to the C601A cat head, another strand 13 is as reclaiming solvent extraction.Logistics 14 through with logistics 10 heat exchange after material 15 enter C601B middle part, C601B cat head gas phase 16 is divided into two strands after the E603 condensation, one material 17 is back to the C601B cat head, another strand 18 is as reclaiming solvent extraction.Logistics 13,18 mixing back materials 20 return C401 and use as solvent cycle after cooling.C601B tower still E604 adopts steam, thermal oil or the heating of other thermals source.
The thick TMP material 19 that C601B tower still removes behind most solvents enters thin-film evaporator E605, and E605 adopts steam, thermal oil or the heating of other thermals source.E605 evaporated on top gas phase 20 enters the demist jar, and after demist, condensation, liquid phase 21 is returned E605, and gaseous condensate 23 enters TMP rectifying tower C602.E605 bottom discharges material 22 is salinity and heavy constituent.Demist jar and E605 evaporation gas phase condenser can resemble the integral structure that is designed to shown in the drawings, also can be 2 separate equipment, adopt pipe connection.
Gaseous condensate 23 enters TMP rectifying tower C602, C602 preferred separator tower structure, and by dividing plate one side charging, dividing plate opposite side extraction material 24 is the TMP product.C602 tower still adopts steam, thermal oil or the heating of other thermals source.C602 cat head extraction material 25 is a light constituent, wherein contains part TMP.C602 tower still extraction material 26 is heavy constituent, wherein contains part TMP.
Logistics 25 enters light constituent TMP recovery tower C603, and C603 cat head material 27 is a light constituent.Logistics 26 enters heavy constituent TMP recovery tower C604, and C604 tower still material 30 is heavy constituent.C603 tower still material 28 and C604 cat head material 29 are for reclaiming TMP, and the two mixture 31 returns TMP rectifying tower C602, to improve the TMP product yield.
Below by concrete Application Example the present invention is made an explanation, but for illustrative purposes only rather than the restriction the present invention.
Embodiment
In sodium hydroxide catalysis aldol condensation, and further intersect TriMethylolPropane(TMP) (hereinafter to be referred as the TMP) solution that Connizzaro (Connizzaro) reaction obtains by butyraldehyde-n and formaldehyde, its classical group becomes water 48%, light constituent 0.8%, TMP
30%, heavy constituent 2.5%, sodium formiate and other heavy constituent 18.7% (form in this patent and be mass percent).The employing octanol is an extraction agent, solvent and extraction agent volume ratio 2.2: 1, and 65 ℃ of extraction temperature, pressure 0.1Mpa, the counter-current extraction reaction gained TMP aqueous solution in extraction tower, the extraction cat head is an extracted organic phase, the tower still is a brine waste.
The organic phase that adopts 65 ℃ of clear water, pressure 0.1Mpa in water wash column, to wash the extraction gained then, washing Tata still raffinate water (containing a small amount of salinity) returns the solvent extraction top of tower, and the water wash column cat head obtains salt-free substantially TMP and solvent mixture.Wash water and organic phase volume ratio are 0.1: 1.
Remove solvent through the concentrated TMP after above-mentioned extraction dehydration, the washing desalination at solvent recovery tower A (working pressure 0.1Mpa) and solvent recovery tower B (working pressure 0.05Mpa), obtain solvent and be lower than 2% thick TMP crude product, its classical group becomes octanol 1.5%, light constituent 2.5%, TMP 88.6%, heavy constituent 7.4%.
Above-mentioned TMP crude product under 0.004Mpa with the 0.3kg/h flow through evaporator evaporation, gas-phase feed is to the TMP rectifying tower.TMP rectifying tower diameter 50mm adorns 3 sections diameter 4mm θ ring fillers, top 0.2m, middle part 0.8m, the following 0.45m of charging in the tower.The TMP rectifying tower is operated under 0.001Mpa, quantity of reflux 0.37kg/h, and by extracting the TMP product between the two sections fillers in charging top out, flow is 0.25kg/h.The TMP product purity is greater than 99%, and look number is lower than 15, and yield is greater than 93%.
The heavy constituent TriMethylolPropane(TMP) recovery tower that is not provided for the light constituent TriMethylolPropane(TMP) recovery tower of TMP rectifying tower cat head light constituent among the comparative example and is used for the heavy constituent of TMP rectifying Tata still, so yield is on the low side.If above-mentioned 2 TriMethylolPropane(TMP) recovery towers are set, TMP refining system total recovery can reach more than 98%.

Claims (9)

1, a kind of processing method of refining trimethylolpropane, under alkaline condition, carry out the catalysis aldol reaction by butyraldehyde-n and formaldehyde, and further cross Connizzaro reaction obtains TriMethylolPropane(TMP) solution, it is characterized in that this processing method is that described TriMethylolPropane(TMP) solution is taken off weight, high vacuum rectification and recycling step through concentrated, desalination, solvent recuperation, flash distillation;
1) described concentrate is to adopt single vaporization or multistage evaporation process to finish concentrating of TriMethylolPropane(TMP) solution, removes the most of moisture content in the solution, and formaldehyde, methyl alcohol light constituent;
2) described desalination is to adopt the organic solvent multi-stage counter current extraction, removes moisture content and salinity contained in the thick TriMethylolPropane(TMP) solution, and water is as extraction agent again, and the further desalination of TriMethylolPropane(TMP) solution concentration liquid is finished in washing through multi-stage countercurrent;
3) described solvent recuperation is the purpose that the two tower differential pressures operation of solvent pairs recovery tower in the employing system reaches the integrated operation of economic benefits and social benefits heat, realizes solvent recuperation;
4) to take off heavily be the vaporization that utilizes heat-exchanger rig to finish to remove the thick TriMethylolPropane(TMP) product behind the solvent in described flash distillation, liquid phase is discharged remaining salinity and part heavy constituent, thick TriMethylolPropane(TMP) gas phase enters follow-up TriMethylolPropane(TMP) rectifying tower with liquid form after demist, condensation;
5) described high vacuum rectification is to utilize rectifying tower to operate under high vacuum, adopts the partitioned column structure, and thick TriMethylolPropane(TMP) enters dividing plate one side, the removed overhead light constituent, and the tower still is discharged heavy constituent, by tower middle part, dividing plate opposite side extraction TriMethylolPropane(TMP) product;
6) described recycling step is to utilize rectifying tower to handle TriMethylolPropane(TMP) rectifying tower cat head and tower still material respectively, reclaims wherein contained TriMethylolPropane(TMP).
2, according to the described processing method of claim 1, it is characterized in that described organic solvent is the alcohol organic solvent that contains 5~9 carbon atoms, described organic solvent is the independent a kind of or mixture of above-mentioned multiple solvent.
3, according to the described processing method of claim 1, it is characterized in that the condition of described organic solvent extraction operating process is: 0.05~1.0Mpa, 40~100 ℃.
4, according to the described processing method of claim 1, it is characterized in that the condition of described multi-stage countercurrent washing operating process is: 0.05~1.0Mpa, 30~90 ℃.
5,, it is characterized in that described TriMethylolPropane(TMP) rectifying tower adopts the conventional rectification tower structure, extracts the TriMethylolPropane(TMP) product out by a certain position side line more than the charging according to the described processing method of claim 1.
, according to the described processing method of claim 1, it is characterized in that it is the recovery tower that TriMethylolPropane(TMP) rectifying tower cat head and tower still material are set simultaneously that described TriMethylolPropane(TMP) reclaims, and perhaps only is provided with a certain recovery tower in them.
7,, it is characterized in that described TriMethylolPropane(TMP) rectifying tower is to adopt plate ripple arranged packing or screen waviness structured packing according to the described processing method of claim 1.
8,, it is characterized in that described TriMethylolPropane(TMP) rectifying tower is a liquid phase feeding according to the described processing method of claim 1.
9, according to the described processing method of claim 1, it is characterized in that described solvent recovery step adopts the integrated technological process of double tower heat to be: a solvent recovery tower overhead vapours is used for to another solvent recovery tower charging or a certain position heating of tower middle part, to reduce the operation energy consumption of solvent recuperation.
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CN102617285A (en) * 2012-03-09 2012-08-01 湖北三江化工有限责任公司 Method for generating trimethylolpropane by condensation of formaldehyde and n-butyl alcohol
CN109369333A (en) * 2018-11-27 2019-02-22 濮阳市永安化工有限公司 The method of trimethylolpropane is isolated from trimethylolpropane light component
CN110372475A (en) * 2019-08-16 2019-10-25 南通百川新材料有限公司 A kind of synthesis technology of Low acid high yield trimethylolpropane
CN110511131B (en) * 2019-08-27 2022-08-09 扬州易奇维科技有限公司 Method for preparing beta-hydroxyaldehyde by reactive distillation

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DE10058303A1 (en) * 2000-11-24 2002-05-29 Basf Ag Removal of trialkylammonium formate from polyhydric alcohols, especially trimethylolpropane, comprises treatment with a strongly basic ion exchanger and distillation
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Publication number Priority date Publication date Assignee Title
DE2057352A1 (en) * 1969-11-28 1971-06-16 Koei Chemical Co Process for purifying trimethylolpropane
US3776963A (en) * 1971-03-16 1973-12-04 Celanese Corp Trimethylolpropane recovery
CN1076185A (en) * 1993-01-08 1993-09-15 北京市助剂研究所 The TriMethylolPropane(TMP) production technique is improved
CN1263081A (en) * 1998-12-25 2000-08-16 三菱瓦斯化学株式会社 Method for producing high-purity trimethylopropane
US20020189926A1 (en) * 1999-12-28 2002-12-19 Matthias Dernbach Method for purifying trimethylolpropane, which is produced by hydrogenation, by means of continuous distillation
DE10058303A1 (en) * 2000-11-24 2002-05-29 Basf Ag Removal of trialkylammonium formate from polyhydric alcohols, especially trimethylolpropane, comprises treatment with a strongly basic ion exchanger and distillation

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