CN102304023A - Separation technique of pentaerythritol - Google Patents
Separation technique of pentaerythritol Download PDFInfo
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- CN102304023A CN102304023A CN201110307544A CN201110307544A CN102304023A CN 102304023 A CN102304023 A CN 102304023A CN 201110307544 A CN201110307544 A CN 201110307544A CN 201110307544 A CN201110307544 A CN 201110307544A CN 102304023 A CN102304023 A CN 102304023A
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- pentaerythritol
- tetramethylolmethane
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Abstract
The invention relates to a separation technique, particularly a separation technique of pentaerythritol, which comprises the following steps: 1. carrying out continuous circulation synthesis technique with high temperature and high formaldehyde ratio; 2. carrying out pressurized hydrolysis technique under acidic conditions, thereby decomposing pentaerythritol acetals generated in the reaction process; 3. decolorizing the crude product pentaerythritol solution with activated carbon, removing sodium formate and other impurities with ion exchange resin, and recrystallizing to remove poly-pentaerythritol and other byproducts, thereby further enhancing the product purity and obtaining high-purity pentaerythritol of which the content is 99%. By using the invention, the pentaerythritol can be concentrated to the required concentration in the shortest time, thereby maximally reducing the decomposition action of high temperature on the pentaerythritol and greatly reducing labor intensity of operation of the workers; and the technique provided by the invention is continuous and stable.
Description
Technical field:
The present invention relates to a kind of separating technology, be specifically related to a kind of separating technology of tetramethylolmethane.
Background technology:
Tetramethylolmethane chemical name 2,2-dihydroxymethyl-1, ammediol is the tetravalent alcohol of typical neopentyl structure, has the typical chemical property of polyvalent alcohol, can carry out the various reactions that polyvalent alcohol can be participated in, like nitrated, oxidation, etherificate, esterification, halo etc.
Tetramethylolmethane is the important source material of oil, chemical industry, light industry; Can be used for making siccative oil, aircraft oil, anti-flaming dope, oil freezing point depressant, pentaerythritol epoxy resin, penton engineering materials etc., is that the trinitrol of raw material manufacturing is high explosive explosive with the tetramethylolmethane; The coating that adds tetramethylolmethane can improve luminance brightness, thermotolerance, is widely used in oil, chemistry painting industry industry, for development oil, chemical industry, light industry significance is arranged.China's tetramethylolmethane is mainly used in phthalic resin coating, ucon oil, rosin ester, appropriate youngster's grease, nitro-pentaerythrite, tensio-active agent, softening agent, foodstuff additive, medicine and explosive etc.; Also replace glycerine to use, particularly produce the pure and mild polyether glycol of polyester polyols in multiple occasion.
Whole world tetramethylolmethane manufacturing enterprise is about 40 families altogether, 28 families of ordinary production wherein, and Chinese 12 families account for 43%.Global output was 49.5 ten thousand tons in 2007, and wherein China's Mainland output is 130,000 tons, and ultimate production accounts for the whole world 26%.This proves absolutely that there is the possibility of shuffling in Chinese tetramethylolmethane industry; Along with holding of the 2008 Beijing Olympic Games and Shanghai World's Fair in 2010, government will more and more pay attention to environment protection.The small chemical industry that productivity is low, environmental pollution is serious will be eliminated, and scale enterprise is bound to benefit from it, the market share can be more and more concentrated to major company, and this should change just and strategic partners expected.Coating industry internationalization major company lands China one after another, certainly will build more bridges that move towards the market abroad more, and suitableization will be maximum winner.
China's tetramethylolmethane is mainly used in the production Synolac, in fields such as urethane, rosin ester, lubricating oil, surfactivity chaste tree, softening agent, medicine and explosives application is arranged also in addition.The apparent consumption of tetramethylolmethane in 2007 is about I3 ten thousand t.Wherein, Synolac to the consumption of tetramethylolmethane account for aggregate consumption 64%, lubricating oil accounts for 6%, urethane accounts for 7%, rosin ester accounts for 6%, other field accounts for 16%.
At other field, tetramethylolmethane can be used for aspects such as medicine, agricultural chemicals, daily use chemicals.Present domestic tetramethylolmethane deep processing development Showed Very Brisk.Other fields such as medicine consumed about 2.5 ten thousand t of tetramethylolmethane altogether in 2007, expected the demand to tetramethylolmethane in 2010 and will reach 30,000 t.
According to up-to-date expectation, China in 2010 will reach 200,000 t to the aggregate demand of tetramethylolmethane.Wherein, the consumption ratio in the Synolac field will descend to some extent, and at lubricating oil, the consumption ratio of rosin ester and polyurethane field will rise to some extent.Lubricating oil, rosin ester and polyurethane field are not only higher to the tetramethylolmethane specification of quality simultaneously, and will increase fast the demand of dipentaerythritol and tripentaerythritol.14000 yuan/ton of present 98% tetramethylolmethane market value, dipentaerythritol price be at 33000 yuan/ton, and 95% tetramethylolmethane market value 11000-11500 unit/ton only.Therefore, China's tetramethylolmethane should improve the quality of products, class, enlarge on the range of product and work hard.
On the other hand; Though the tetramethylolmethane that should change has been the device that output in domestic is maximum, consumption is minimum, profit is best; But the tetramethylolmethane quality can not satisfy the requirement of domestic market to high-quality tetramethylolmethane; Be subjected to the influence of external high-quality tetramethylolmethane; 86%, 92%, 95% technical grade pentaerythritol market atrophy day by day; Price day by day reduces, and profit is not high.The high purity monopentaerythritol of exploitation 98% above content is the main direction of Future Development.
Domestic present operation evaporation technology is the intermittent type evaporation, and the fluctuation of quality product is bigger, can't satisfy the requirement that high-quality tetramethylolmethane is produced.Because tetramethylolmethane is a heat-sensitive substance, at high temperature decompose easily, this has not only reduced the yield of tetramethylolmethane, and the degree of staining of tetramethylolmethane is increased, and has reduced the quality of tetramethylolmethane.
Summary of the invention:
The separating technology that the purpose of this invention is to provide tetramethylolmethane; It can make the tetramethylolmethane can be in the shortest time concentration to requiring concentration; Thereby reduced the Decomposition of high temperature to greatest extent to tetramethylolmethane, and can be continual and steady, the labour intensity of workman's operation also greatly reduced simultaneously.
In order to solve the existing problem of background technology, the present invention adopts following technical scheme: its separating technology is: the continuous circulation synthesis technique that 1, adopts the high formaldehyde proportioning of high temperature; 2, adopt pressurized hydrolysis technology under the acidic conditions,, the tetramethylolmethane acetals that generates in the reaction process is decomposed through hydrolysis; 3, the decolouring of crude product tetramethylolmethane solution, removal of impurities are further purified; After removing impurity, recrystallization such as sodium formiate through activated carbon decolorizing, ion exchange resin and removing byproduct such as many tetramethylolmethanes; Product purity further improves, and reaches 99% monopentaerythritol of high purity thereby can obtain content.
Adopt in the described separating technology 1 that actual formaldehyde proportioning is 10: 15 in the reaction process of continuous circulation synthesis technique of the high formaldehyde proportioning of high temperature, can guarantee the highly selective of monopentaerythritol.
The present invention has following beneficial effect: can make the tetramethylolmethane can be in the shortest time concentration to requiring concentration; Thereby reduced the Decomposition of high temperature to greatest extent to tetramethylolmethane; And can be continual and steady, also greatly reduce the labour intensity of workman's operation simultaneously.
Embodiment:
This embodiment adopts following technical scheme: its separating technology is: the continuous circulation synthesis technique that 1, adopts the high formaldehyde proportioning of high temperature; 2, adopt pressurized hydrolysis technology under the acidic conditions,, the tetramethylolmethane acetals that generates in the reaction process is decomposed through hydrolysis; 3, the decolouring of crude product tetramethylolmethane solution, removal of impurities are further purified; After removing impurity, recrystallization such as sodium formiate through activated carbon decolorizing, ion exchange resin and removing byproduct such as many tetramethylolmethanes; Product purity further improves, and reaches 99% monopentaerythritol of high purity thereby can obtain content.
Adopt in the described separating technology 1 that actual formaldehyde proportioning is 10: 15 in the reaction process of continuous circulation synthesis technique of the high formaldehyde proportioning of high temperature, can guarantee the highly selective of monopentaerythritol.
This embodiment can make the tetramethylolmethane can be in the shortest time concentration to requiring concentration, thereby has reduced the Decomposition of high temperature to tetramethylolmethane to greatest extent, and can be continual and steady, also greatly reduce the labour intensity of workman's operation simultaneously.
Claims (2)
1. the separating technology of tetramethylolmethane is characterized in that its separating technology is: the continuous circulation synthesis technique that 1, adopts the high formaldehyde proportioning of high temperature; 2, adopt pressurized hydrolysis technology under the acidic conditions,, the tetramethylolmethane acetals that generates in the reaction process is decomposed through hydrolysis; 3, the decolouring of crude product tetramethylolmethane solution, removal of impurities are further purified; After removing impurity, recrystallization such as sodium formiate through activated carbon decolorizing, ion exchange resin and removing byproduct such as many tetramethylolmethanes; Product purity further improves, and reaches 99% monopentaerythritol of high purity thereby can obtain content.
2. the separating technology of tetramethylolmethane according to claim 1 is characterized in that adopting in the described separating technology 1 that actual formaldehyde proportioning is 10: 15 in the reaction process of continuous circulation synthesis technique of the high formaldehyde proportioning of high temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110307544A CN102304023A (en) | 2011-10-12 | 2011-10-12 | Separation technique of pentaerythritol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110307544A CN102304023A (en) | 2011-10-12 | 2011-10-12 | Separation technique of pentaerythritol |
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| CN102304023A true CN102304023A (en) | 2012-01-04 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201110307544A Pending CN102304023A (en) | 2011-10-12 | 2011-10-12 | Separation technique of pentaerythritol |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103450001A (en) * | 2013-09-23 | 2013-12-18 | 湖北宜化化工股份有限公司 | Method and equipment for concentrating sodium formate in pentaerythritol production |
| CN108658729A (en) * | 2018-06-19 | 2018-10-16 | 濮阳市永安化工有限公司 | Waste active carbon recycles the device and its recovery method of pentaerythrite |
| CN109503325A (en) * | 2018-12-10 | 2019-03-22 | 安徽金禾实业股份有限公司 | A kind of method that pentaerythrite reduces coloration |
| CN115784844A (en) * | 2022-12-08 | 2023-03-14 | 赤峰瑞阳化工有限公司 | Method for recovering formaldehyde and methanol and removing macromolecular impurities by pentaerythritol multi-tower series high-efficiency rectification |
-
2011
- 2011-10-12 CN CN201110307544A patent/CN102304023A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103450001A (en) * | 2013-09-23 | 2013-12-18 | 湖北宜化化工股份有限公司 | Method and equipment for concentrating sodium formate in pentaerythritol production |
| CN108658729A (en) * | 2018-06-19 | 2018-10-16 | 濮阳市永安化工有限公司 | Waste active carbon recycles the device and its recovery method of pentaerythrite |
| CN109503325A (en) * | 2018-12-10 | 2019-03-22 | 安徽金禾实业股份有限公司 | A kind of method that pentaerythrite reduces coloration |
| CN109503325B (en) * | 2018-12-10 | 2021-12-21 | 安徽金禾实业股份有限公司 | Method for reducing chroma of pentaerythritol |
| CN115784844A (en) * | 2022-12-08 | 2023-03-14 | 赤峰瑞阳化工有限公司 | Method for recovering formaldehyde and methanol and removing macromolecular impurities by pentaerythritol multi-tower series high-efficiency rectification |
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Application publication date: 20120104 |
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