CN102115367A - Method for preparing pentaerythritol as well as cobaltous formate and sodium chloride - Google Patents
Method for preparing pentaerythritol as well as cobaltous formate and sodium chloride Download PDFInfo
- Publication number
- CN102115367A CN102115367A CN2010106106232A CN201010610623A CN102115367A CN 102115367 A CN102115367 A CN 102115367A CN 2010106106232 A CN2010106106232 A CN 2010106106232A CN 201010610623 A CN201010610623 A CN 201010610623A CN 102115367 A CN102115367 A CN 102115367A
- Authority
- CN
- China
- Prior art keywords
- sodium
- tetramethylolmethane
- filtrate
- pentaerythritol
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a method for preparing pentaerythritol as well as cobaltous formate and sodium chloride. The method comprises the following steps: waste liquor generated during the production of pentaerythritol through condensation of formaldehyde and acetaldehyde is distilled under reduced pressure to obtain a saturated pentaerythritol solution, the saturated pentaerythritol solution is then cooled, and pentaerythritol crystals and a filtrate I are obtained through filtering separation; the filtrate I is distilled under reduced pressure into a saturated sodium formate solution, the saturated sodium formate solution is cooled, and sodium formate crystals and a filtrate II are obtained after sodium formate is separated through crystallization; the pentaerythritol crystals are washed, dried and crushed into pentaerythritol products; the sodium formate crystals are dissolved in water and then react with a cobaltous chloride solution to obtain a solution containing cobaltous formate and sodium chloride, and then the solution is filtered to obtain few filter cake impurities and a clear filtrate III; and the filtrate III is distilled, cooled and separated by crystallization to obtain a mixed product of cobaltous 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 cobaltous 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 make 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 is under condition of stirring and 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 filtrate 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.With volume calculation unit 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 cobaltous 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, cobaltous formate and sodium-chlor, make full use of formaldehyde and acetaldehyde condensation and produced the potential value of tetramethylolmethane gained waste liquid, and do not produce secondary pollution, being one turns waste into wealth, economic and practical method.
Technical scheme of the present invention is as follows: a kind of method for preparing tetramethylolmethane coproduction cobaltous 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 after filtration, obtains crystals of pentaerythritol and filtrate one; Filtrate one further underpressure distillation is the sodium formiate saturated solution, and postcooling, the sodium formiate crystallization is separated out, and is separating after filtration, obtains sodium formiate crystal and filtrate 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 cobalt chloride then: the 0.8-1.2 reaction with cobalt chloride solution, obtain containing the solution of cobaltous formate and sodium-chlor, after filtration, obtain extremely a spot of filter cake impurity and clarifying filtrate three;
Step D: filtrate three is through distillation, and cooling, crystallization are separated out, and obtain cobaltous formate and sodium-chlor mixing prod.
The method for preparing tetramethylolmethane coproduction formic acid and sodium-chlor of the present invention, its chemical equation:
2HCOONa+CoCl
2＝＝＝＝Co(COOH)
2+2NaCl
Beneficial effect of the present invention is: the method for preparing tetramethylolmethane coproduction cobaltous formate and sodium-chlor of the present invention, formaldehyde and acetaldehyde condensation are produced tetramethylolmethane gained waste liquid through simple processing treatment, make tetramethylolmethane coproduction cobaltous formate and sodium-chlor, make full use of formaldehyde and acetaldehyde condensation and produced the potential value of tetramethylolmethane gained waste liquid, and do not produce 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 cobaltous 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 after filtration, obtains crystals of pentaerythritol and filtrate one; Filtrate one further underpressure distillation is the sodium formiate saturated solution, and postcooling, the sodium formiate crystallization is separated out, and is separating after filtration, obtains sodium formiate crystal and filtrate 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 cobalt chloride solution, obtain containing the solution of cobaltous formate and sodium-chlor, after filtration, obtain containing the solution of cobaltous formate and sodium-chlor, after filtration, obtain extremely a spot of filter cake impurity and clarifying filtrate three;
Step D: filtrate three is through distillation, and cooling, crystallization are separated out, and obtain cobaltous formate and sodium-chlor mixing prod, and the quality of the pure substance of the cobaltous formate that it contains is 149kg; 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 cobaltous 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 after filtration, obtains crystals of pentaerythritol and filtrate one; Filtrate one further underpressure distillation is the sodium formiate saturated solution, and postcooling, the sodium formiate crystallization is separated out, and is separating after filtration, obtains sodium formiate crystal and filtrate 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 cobalt chloride solution, obtain containing the solution of cobaltous formate and sodium-chlor, after filtration, obtain extremely a spot of filter cake impurity and clarifying filtrate three;
Step D: filtrate three is through distillation, and cooling, crystallization are separated out, and obtain cobaltous formate and sodium-chlor mixing prod, and the quality of the pure substance of the cobaltous formate that it contains is 149kg; 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 cobaltous 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 after filtration, obtains crystals of pentaerythritol and filtrate one; Filtrate one further underpressure distillation is the sodium formiate saturated solution, and postcooling, the sodium formiate crystallization is separated out, and is separating after filtration, obtains sodium formiate crystal and filtrate 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 cobalt chloride solution, obtain containing the solution of cobaltous formate and sodium-chlor, after filtration, obtain extremely a spot of filter cake impurity and clarifying filtrate three;
Step D: filtrate three is through distillation, and cooling, crystallization are separated out, and obtain cobaltous formate and sodium-chlor mixing prod, and the quality of the pure substance of the cobaltous formate that it contains is 119.2kg; The quality of the pure substance of the sodium-chlor that it contains is 93.6kg.
Above content be in conjunction with concrete preferred implementation to further describing that the present invention did, can not assert that concrete enforcement of the present invention is confined to these explanations.For the general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, its framework form can be flexible and changeable, can the subseries product.Just make some simple deduction or replace, all should be considered as belonging to the scope of patent protection that the present invention is determined by claims of being submitted to.
Claims (1)
1. a method for preparing tetramethylolmethane coproduction cobaltous 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 after filtration, obtains crystals of pentaerythritol and filtrate one; Filtrate one further underpressure distillation is the sodium formiate saturated solution, and postcooling, the sodium formiate crystallization is separated out, and is separating after filtration, obtains sodium formiate crystal and filtrate 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 1 with the ratio of the molar content of the pure substance of sodium formiate and cobalt chloride then: the 0.8-1.2 reaction with cobalt chloride solution, obtain containing the solution of cobaltous formate and sodium-chlor, after filtration, obtain extremely a spot of filter cake impurity and clarifying filtrate three;
Step D: filtrate three is through distillation, and cooling, crystallization are separated out, and obtain cobaltous formate and sodium-chlor mixing prod.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106106232A CN102115367A (en) | 2010-12-29 | 2010-12-29 | Method for preparing pentaerythritol as well as cobaltous formate and sodium chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106106232A CN102115367A (en) | 2010-12-29 | 2010-12-29 | Method for preparing pentaerythritol as well as cobaltous formate and sodium chloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102115367A true CN102115367A (en) | 2011-07-06 |
Family
ID=44214310
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010106106232A Pending CN102115367A (en) | 2010-12-29 | 2010-12-29 | Method for preparing pentaerythritol as well as cobaltous formate and sodium chloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102115367A (en) |
-
2010
- 2010-12-29 CN CN2010106106232A patent/CN102115367A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102115407B (en) | Method for producing co-product of pentaerythritol as well as potassium formate and sodium sulfate | |
| CN102115419A (en) | Method for preparing pentaerythritol as well as lithium formate and sodium chloride | |
| CN102115394B (en) | Method for preparing pentaerythritol with co-production of strontium formate and sodium chloride | |
| CN102115406A (en) | Method for preparing pentaerythritol as well as formic acid and sodium nitrate | |
| CN102115401A (en) | Method for preparing pentaerythritol as well as formic acid and sodium sulfide | |
| CN102115367A (en) | Method for preparing pentaerythritol as well as cobaltous formate and sodium chloride | |
| CN102115413A (en) | Method for preparing pentaerythritol and coproducing calcium formate and sodium chloride | |
| CN102115408B (en) | Method for preparing pentaerythritol with co-production of potassium formate and sodium carbonate | |
| CN102115420B (en) | Method for preparing pentaerythritol and co-producing potassium formate and sodium phosphate | |
| CN102115411A (en) | Method for preparing pentaerythritol as well as manganese formate and sodium chloride | |
| CN102115412A (en) | Method for preparing pentaerythritol and co-producing zinc formate and sodium chloride | |
| CN102115395A (en) | Method for producing co-product of pentaerythritol as well as ammonium formate and sodium chloride | |
| CN102115397A (en) | Method for preparing pentaerythritol and coproducing cobalt formate and sodium sulfide | |
| CN102115393A (en) | Method for producing co-product of pentaerythritol as well as potassium formate and sodium hydroxide | |
| CN102115424A (en) | Method for preparing pentaerythritol and co-producing manganese formate and sodium phosphate | |
| CN102115414A (en) | Method for preparing pentaerythritol with co-production of manganese formate and sodium sulfide | |
| CN102115368A (en) | Method for preparing pentaerythritol, ammonium formate and sodium sulfide | |
| CN102115387A (en) | Method for preparing pentaerythritol and coproducing antimony formate and sodium sulfide | |
| CN102115398A (en) | Method for preparing pentaerythritol and co-producing magnesium formate and sodium sulfide | |
| CN102115396A (en) | Method for preparing pentaerythritol and coproducing strontium formate and sodium sulfide | |
| CN102115410A (en) | Method for preparing pentaerythritol as well as zinc formate and sodium carbonate | |
| CN102115409A (en) | Method for preparing pentaerythritol as well as magnesium formate and sodium carbonate | |
| CN102115364A (en) | Method for preparing pentaerythritol, and co-producing manganese formate and sodium carbonate | |
| CN102115405A (en) | Method for preparing pentaerythritol as well as ammonium formate and sodium carbonate | |
| CN102115404A (en) | Method for preparing pentaerythritol with co-production of formic acid and sodium phosphate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20110706 |