CN102115394B - Method for preparing pentaerythritol with co-production of strontium formate and sodium chloride - Google Patents
Method for preparing pentaerythritol with co-production of strontium formate and sodium chloride Download PDFInfo
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- CN102115394B CN102115394B CN2010106112498A CN201010611249A CN102115394B CN 102115394 B CN102115394 B CN 102115394B CN 2010106112498 A CN2010106112498 A CN 2010106112498A CN 201010611249 A CN201010611249 A CN 201010611249A CN 102115394 B CN102115394 B CN 102115394B
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- tetramethylolmethane
- sodium
- pentaerythritol
- strontium
- formate
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Abstract
The invention provides a method for preparing pentaerythritol with the co-production of strontium formate and sodium chloride. The method comprises the following steps of: decompressing and distilling waste liquod, obtained by the condensation production of pentaerythritol from formaldehyde and acetaldehyde, into a saturated pentaerythritol solution, cooling, filtering and separating to obtain a pentaerythritol crystal and a filtrate (1); decompressing and distilling the filtrate (1) to obtain a saturated sodium formate solution, cooling, crystallizing and separating out sodium formate to obtain a sodium formate crystal and a filtrate (2); washing, drying and crushing the pentaerythritol crystal to obtain a pentaerythritol product; dissolving the sodium formate crystal in water, reacting with a strontium chloride solution to obtain a solution containing strontium formate and sodium chloride, and filtering to obtain a minute quantity of filter cake impurities and a clear filtrate (3); and distilling the filtrate (3), and cooling and crystallizing for separating crystals out to obtain the mixed product of strontium formate and sodium chloride.
Description
Technical field
The present invention relates to the organic chemical industry and produce the improvement of tetramethylolmethane gained waste liquid and the technical field of utilization, especially a kind of method for preparing tetramethylolmethane coproduction strontium formate and sodium-chlor, its raw material is for producing tetramethylolmethane gained waste liquid.
Background technology
Tetramethylolmethane is a kind of organic intermediate of having many uses, and is usually used in coatings industry, is the raw material of alkydpaints, and hardness, glossiness and the weather resistance of paint film are improved; Also be used as the abietinic raw materials such as printing-ink of varnish, colored paint, and can make the coating of flame retardant resistance, siccative oil and aero oil lubricate wet goods.Be that to process the tetramethylolmethane tetranitrate be volatile explosive to raw material with the tetramethylolmethane.The sour fat of tetramethylolmethane fat can be made the softening agent and the stablizer of polyvinyl chloride resin, in addition, also can be used for medicine, agricultural chemicals and lubricated wet goods manufacturing.
Tetramethylolmethane is to be raw material with formaldehyde and acetaldehyde, and condensation makes in the presence of basic catalyst.Be exactly specifically: 37% formaldehyde under condition of stirring with sodium hydroxide and acetaldehyde; Slowly be warming up to 25-32 degree centigrade with steam; Keeping this temperature stirred 6-7 hour; The sulfuric acid that adds with mole folding hundred such as sodium hydroxide neutralizes, and the filtrating vapourisation under reduced pressure is concentrated, crystallization, filtration and drying make finished product.
Produce tetramethylolmethane gained waste liquid and come the mother liquor and the washing water of inherent filtration and washing.Contain sodium formiate 25%, tetramethylolmethane 6-8%, other organic substances 15% in the mother liquor.One ton of tetramethylolmethane of every production has 3 cubic metres of crystalline mother solutions to discharge approximately.If by yield 80%, one ton of tetramethylolmethane of then every production is wanted 0.6 ton of by-product sodium formiate.Use volume calculation unit to be: the sodium formiate volume content is 300-500 (g/L), tetramethylolmethane volume content 50-100 (g/L), and the mother liquor quantity discharged of producing product per ton is the 2-3 ton.
Discharge arbitrarily or abandon if produce tetramethylolmethane gained waste liquid,, also waste raw material, for this reason, be necessary to explore the comprehensive regulation and methods for using them of producing tetramethylolmethane gained waste liquid without influencing environment.
Summary of the invention
Produce tetramethylolmethane with formaldehyde and acetaldehyde condensation, contain sodium formiate 25wt.%, tetramethylolmethane 6-8wt.%, other organic substances 15wt.% in the gained waste liquid.For to its comprehensive regulation and application, the invention provides a kind of method for preparing tetramethylolmethane coproduction strontium formate and sodium-chlor, its raw material is that formaldehyde and acetaldehyde condensation are produced tetramethylolmethane gained waste liquid.This method; Formaldehyde and acetaldehyde condensation are produced tetramethylolmethane gained waste liquid through simple processing treatment; Make tetramethylolmethane, strontium formate and sodium-chlor, made full use of the potential value that formaldehyde and acetaldehyde condensation are produced tetramethylolmethane gained waste liquid, and do not produced secondary pollution; Being one turns waste into wealth, economic and practical method.
Technical scheme of the present invention is following: a kind of method for preparing tetramethylolmethane coproduction strontium formate and sodium-chlor, its raw material are that formaldehyde and acetaldehyde condensation are produced tetramethylolmethane gained waste liquid, comprise the steps:
Steps A: is the tetramethylolmethane saturated solution with formaldehyde and acetaldehyde condensation production tetramethylolmethane gained waste liquid through underpressure distillation, and postcooling, the tetramethylolmethane crystallization is separated out, and separates through filtering, and obtains crystals of pentaerythritol and filtrates one; Filtrating one further underpressure distillation is the sodium formiate saturated solution, and postcooling, the sodium formiate crystallization is separated out, and is separating through filtering, and obtains sodium formiate crystal and filtrating two;
Step B: the above-mentioned crystals of pentaerythritol that obtains through washing, dry and pulverizing, is obtained the tetramethylolmethane product;
Step C: the above-mentioned sodium formiate crystal that obtains is water-soluble; It is 2 with the ratio of the molar content of the pure substance of sodium formiate and strontium chloride then: the 0.8-1.2 reaction with strontium chloride solution; Obtain containing the solution of strontium formate and sodium-chlor,, obtain extremely a spot of filter cake impurity and clarifying filtrating three through filtering;
Step D: filtrating three is through distillation, and cooling, crystallization are separated out, and obtain strontium formate and sodium-chlor mixing prod.
The method for preparing tetramethylolmethane coproduction formic acid and sodium-chlor according to the invention, its chemical equation:
2HCOONa+SrCl
2＝＝＝＝Sr(COOH)
2+2NaCl
Beneficial effect of the present invention is: the method for preparing tetramethylolmethane coproduction strontium formate and sodium-chlor according to the invention; Formaldehyde and acetaldehyde condensation are produced tetramethylolmethane gained waste liquid through simple processing treatment; Make tetramethylolmethane coproduction strontium formate and sodium-chlor, made full use of the potential value that formaldehyde and acetaldehyde condensation are produced tetramethylolmethane gained waste liquid, and do not produced secondary pollution; Being one turns waste into wealth, economic and practical method.This method is simple to operate, and facility investment is few, is worthy of popularization.
Embodiment
Embodiment 1:
A kind of method for preparing tetramethylolmethane coproduction strontium formate and sodium-chlor, its raw material are that formaldehyde and acetaldehyde condensation are produced tetramethylolmethane gained waste liquid, and wherein, sodium formiate 25wt.%, tetramethylolmethane 7wt.% comprise the steps:
Steps A: formaldehyde and acetaldehyde condensation are produced tetramethylolmethane gained waste liquid 544kg, are the tetramethylolmethane saturated solution through underpressure distillation, and postcooling, the tetramethylolmethane crystallization is separated out, and separates through filtering, and obtains crystals of pentaerythritol and filtrating one; Filtrating one further underpressure distillation is the sodium formiate saturated solution, and postcooling, the sodium formiate crystallization is separated out, and is separating through filtering, and obtains sodium formiate crystal and filtrating two;
Step B: the above-mentioned crystals of pentaerythritol that obtains through washing, dry and pulverizing, is obtained the tetramethylolmethane product, and the quality of the tetramethylolmethane pure substance that it contains is 38.08kg;
Step C: the above-mentioned sodium formiate crystal that obtains is water-soluble; Be reaction in 2: 1.2 with the ratio of the molar content of the pure substance of sodium formiate and hydrogenchloride then with strontium chloride solution; Obtain containing the solution of strontium formate and sodium-chlor,, obtain containing the solution of strontium formate and sodium-chlor through filtering; Through filtering, obtain extremely a spot of filter cake impurity and clarifying filtrating three;
Step D: filtrating three is through distillation, and cooling, crystallization are separated out, and obtain strontium formate and sodium-chlor mixing prod, and the quality of the pure substance of the strontium formate that it contains is 178kg; The quality of the pure substance of the sodium-chlor that it contains is 117kg.
Embodiment 2:
A kind of method for preparing tetramethylolmethane coproduction strontium formate and sodium-chlor, its raw material are that formaldehyde and acetaldehyde condensation are produced tetramethylolmethane gained waste liquid, and wherein, sodium formiate 25wt.%, tetramethylolmethane 7wt.% comprise the steps:
Steps A: formaldehyde and acetaldehyde condensation are produced tetramethylolmethane gained waste liquid 544kg, are the tetramethylolmethane saturated solution through underpressure distillation, and postcooling, the tetramethylolmethane crystallization is separated out, and separates through filtering, and obtains crystals of pentaerythritol and filtrating one; Filtrating one further underpressure distillation is the sodium formiate saturated solution, and postcooling, the sodium formiate crystallization is separated out, and is separating through filtering, and obtains sodium formiate crystal and filtrating two;
Step B: the above-mentioned crystals of pentaerythritol that obtains through washing, dry and pulverizing, is obtained the tetramethylolmethane product, and the quality of the tetramethylolmethane pure substance that it contains is 38.08kg;
Step C: the above-mentioned sodium formiate crystal that obtains is water-soluble; Be reaction in 2: 1 with the ratio of the molar content of the pure substance of sodium formiate and hydrogenchloride then with strontium chloride solution; Obtain containing the solution of strontium formate and sodium-chlor,, obtain extremely a spot of filter cake impurity and clarifying filtrating three through filtering;
Step D: filtrating three is through distillation, and cooling, crystallization are separated out, and obtain strontium formate and sodium-chlor mixing prod, and the quality of the pure substance of the strontium formate that it contains is 178kg; The quality of the pure substance of the sodium-chlor that it contains is 117kg.
Embodiment 3:
A kind of method for preparing tetramethylolmethane coproduction strontium formate and sodium-chlor, its raw material are that formaldehyde and acetaldehyde condensation are produced tetramethylolmethane gained waste liquid, and wherein, sodium formiate 25wt.%, tetramethylolmethane 7wt.% comprise the steps:
Steps A: formaldehyde and acetaldehyde condensation are produced tetramethylolmethane gained waste liquid 544kg, are the tetramethylolmethane saturated solution through underpressure distillation, and postcooling, the tetramethylolmethane crystallization is separated out, and separates through filtering, and obtains crystals of pentaerythritol and filtrating one; Filtrating one further underpressure distillation is the sodium formiate saturated solution, and postcooling, the sodium formiate crystallization is separated out, and is separating through filtering, and obtains sodium formiate crystal and filtrating two;
Step B: the above-mentioned crystals of pentaerythritol that obtains through washing, dry and pulverizing, is obtained the tetramethylolmethane product, and the quality of the tetramethylolmethane pure substance that it contains is 38.08kg;
Step C: the above-mentioned sodium formiate crystal that obtains is water-soluble; Be reaction in 2: 0.8 with the ratio of the molar content of the pure substance of sodium formiate and hydrogenchloride then with strontium chloride solution; Obtain containing the solution of strontium formate and sodium-chlor,, obtain extremely a spot of filter cake impurity and clarifying filtrating three through filtering;
Step D: filtrating three is through distillation, and cooling, crystallization are separated out, and obtain strontium formate and sodium-chlor mixing prod, and the quality of the pure substance of the strontium formate that it contains is 142.6kg; The quality of the pure substance of the sodium-chlor that it contains is 93.6kg.
Above content is to combine concrete preferred implementation to the further explain that the present invention did, and can not assert that practical implementation of the present invention is confined to these explanations.For the those of ordinary skill of technical field under the present invention, under the prerequisite that does not break away from the present invention's design, its framework form can be flexible and changeable, can the subseries product.Just make some simple deduction or replace, all should be regarded as belonging to the scope of patent protection that the present invention is confirmed by claims of being submitted to.
Claims (1)
1. a method for preparing tetramethylolmethane coproduction strontium formate and sodium-chlor is characterized in that, its raw material is that formaldehyde and acetaldehyde condensation are produced tetramethylolmethane gained waste liquid, comprises the steps:
Steps A: is the tetramethylolmethane saturated solution with formaldehyde and acetaldehyde condensation production tetramethylolmethane gained waste liquid through underpressure distillation, and postcooling, the tetramethylolmethane crystallization is separated out, and separates through filtering, and obtains crystals of pentaerythritol and filtrates one; Filtrating one further underpressure distillation is the sodium formiate saturated solution, and postcooling, the sodium formiate crystallization is separated out, and is separating through filtering, and obtains sodium formiate crystal and filtrating two;
Step B: the above-mentioned crystals of pentaerythritol that obtains through washing, dry and pulverizing, is obtained the tetramethylolmethane product;
Step C: the above-mentioned sodium formiate crystal that obtains is water-soluble; It is 2 with the ratio of the molar content of the pure substance of sodium formiate and strontium chloride then: the 0.8-1.2 reaction with strontium chloride solution; Obtain containing the solution of strontium formate and sodium-chlor,, obtain extremely a spot of filter cake impurity and clarifying filtrating three through filtering;
Step D: filtrating three is through distillation, and cooling, crystallization are separated out, and obtain strontium formate and sodium-chlor mixing prod.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106112498A CN102115394B (en) | 2010-12-29 | 2010-12-29 | Method for preparing pentaerythritol with co-production of strontium formate and sodium chloride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106112498A CN102115394B (en) | 2010-12-29 | 2010-12-29 | Method for preparing pentaerythritol with co-production of strontium formate and sodium chloride |
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| Publication Number | Publication Date |
|---|---|
| CN102115394A CN102115394A (en) | 2011-07-06 |
| CN102115394B true CN102115394B (en) | 2012-07-25 |
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| CN2010106112498A Expired - Fee Related CN102115394B (en) | 2010-12-29 | 2010-12-29 | Method for preparing pentaerythritol with co-production of strontium formate and sodium chloride |
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Non-Patent Citations (1)
| Title |
|---|
| 灵通.季戊四醇废液综合利用.《环境污染与防治》.1989,(第3期),第41页. * |
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