CN102115403A - Method for preparing pentaerythritol and co-producing magnesium formate and sodium phosphate - Google Patents
Method for preparing pentaerythritol and co-producing magnesium formate and sodium phosphate Download PDFInfo
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- CN102115403A CN102115403A CN2010106112835A CN201010611283A CN102115403A CN 102115403 A CN102115403 A CN 102115403A CN 2010106112835 A CN2010106112835 A CN 2010106112835A CN 201010611283 A CN201010611283 A CN 201010611283A CN 102115403 A CN102115403 A CN 102115403A
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Abstract
The invention provides a method for preparing pentaerythritol and co-producing magnesium formate and sodium phosphate. The method comprises the following steps: carrying out reduced pressure distillation on a waste liquid generated by producing pentaerythritol through the condensation of formaldehyde and acetaldehyde to obtain a pentaerythritol saturated solution, cooling, and carrying out filtering separation to obtain a pentaerythritol crystal and a filtrate 1; carrying out reduced pressure distillation on the filtrate 1 to obtain a sodium formate saturated solution, cooling to crystallize and separate out sodium formate to obtain a sodium formate crystal and a filtrate 2; washing, drying and grinding the pentaerythritol crystal to obtain a pentaerythritol product; dissolving the sodium formate crystal in water to react with a magnesium phosphate solution, filtering to obtain a filtrate 3 containing magnesium formate and sodium phosphate; carrying out reduced pressure distillation on the filtrate 3 to obtain a sodium phosphate saturated solution, cooling and carrying out filtering separation to obtain a sodium phosphate crystal and a filtrate 4; carrying out reduced pressure distillation on the filtrate 4 to obtain a magnesium formate supersaturated solution, and cooling to obtain a magnesium formate crystal; and respectively washing, drying and grinding the sodium phosphate crystal and the magnesium formate crystal to respectively obtain a sodium phosphate product and a magnesium formate product.
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 magnesium formiate and sodium phosphate, 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: formic acid ammonium formiate sodium 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 magnesium formiate and sodium phosphate, 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, magnesium formiate and sodium phosphate, 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 magnesium formiate and sodium phosphate, 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, be 6 with the ratio of the molar content of the pure substance of sodium formiate and trimagnesium phosphate then with trimagnesium phosphate solution: the 0.8-1.2 reaction, produce magnesium formiate and sodium phosphate, after filtration, remove a spot of filter residue, obtain containing the filtrate three of magnesium formiate and sodium phosphate;
Step D: filtrate three is the sodium phosphate saturated solution through underpressure distillation, is cooled to 0 ℃, and at this moment, the saturation ratio of sodium phosphate is 4.5g, the saturation ratio of magnesium formiate is 14g, and therefore, the sodium phosphate crystallization is separated out, and magnesium formiate separates still in solution after filtration, obtains sodium phosphate crystal and filtrate four; Filtrate four further underpressure distillation are the magnesium formiate supersaturated solution, are cooled to 0 ℃, and at this moment, the magnesium formiate mass crystallization is separated out, and obtains the magnesium formiate crystal; Sodium phosphate crystal and magnesium formiate crystal advance washing, dry and pulverizing respectively, thereby obtain sodium phosphate product and magnesium formiate product respectively.
The method for preparing tetramethylolmethane coproduction magnesium formiate and sodium phosphate of the present invention, its chemical equation:
6HCOONa+Mg
3(PO
4)
2＝＝＝＝3Mg(COOH)
2+2Na
3PO
4
Beneficial effect of the present invention is: the method for preparing tetramethylolmethane coproduction magnesium formiate and sodium phosphate of the present invention, formaldehyde and acetaldehyde condensation are produced tetramethylolmethane gained waste liquid through simple processing treatment, make tetramethylolmethane coproduction magnesium formiate and sodium phosphate, 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 formic acid and sodium phosphate, 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 816kg, 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; The quality of the tetramethylolmethane pure substance that it contains is 57.12kg;
Step C: the above-mentioned sodium formiate crystal that obtains is water-soluble, be reaction in 6: 1.2 with the ratio of the molar content of the pure substance of sodium formiate and trimagnesium phosphate then, produce magnesium formiate and sodium phosphate, after filtration with trimagnesium phosphate solution, remove a spot of filter residue, obtain containing the filtrate three of magnesium formiate and sodium phosphate;
Step D: filtrate three is the sodium phosphate saturated solution through underpressure distillation, is cooled to 0 ℃, and at this moment, the saturation ratio of sodium phosphate is 4.5g, the saturation ratio of magnesium formiate is 14g, and therefore, the sodium phosphate crystallization is separated out, and magnesium formiate separates still in solution after filtration, obtains sodium phosphate crystal and filtrate four; Filtrate four further underpressure distillation are the magnesium formiate supersaturated solution, are cooled to 0 ℃, and at this moment, the magnesium formiate mass crystallization is separated out, and obtains the magnesium formiate crystal; Sodium phosphate crystal and magnesium formiate crystal advance washing, dry and pulverizing respectively, thereby obtain sodium phosphate product and magnesium formiate product respectively, and the quality of the sodium phosphate pure substance that it contains is 164kg, and the quality of the magnesium formiate pure substance that it contains is 171kg.
Embodiment 2:
A kind of method for preparing tetramethylolmethane coproduction formic acid and sodium phosphate, 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 816kg, 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; The quality of the tetramethylolmethane pure substance that it contains is 57.12kg;
Step C: the above-mentioned sodium formiate crystal that obtains is water-soluble, be reaction in 6: 1 with the ratio of the molar content of the pure substance of sodium formiate and trimagnesium phosphate then, produce magnesium formiate and sodium phosphate, after filtration with trimagnesium phosphate solution, remove a spot of filter residue, obtain containing the filtrate three of magnesium formiate and sodium phosphate;
Step D: filtrate three is the sodium phosphate saturated solution through underpressure distillation, is cooled to 0 ℃, and at this moment, the saturation ratio of sodium phosphate is 4.5g, the saturation ratio of magnesium formiate is 14g, and therefore, the sodium phosphate crystallization is separated out, and magnesium formiate separates still in solution after filtration, obtains sodium phosphate crystal and filtrate four; Filtrate four further underpressure distillation are the magnesium formiate supersaturated solution, are cooled to 0 ℃, and at this moment, the magnesium formiate mass crystallization is separated out, and obtains the magnesium formiate crystal; Sodium phosphate crystal and magnesium formiate crystal advance washing, dry and pulverizing respectively, thereby obtain sodium phosphate product and magnesium formiate product respectively, and the quality of the sodium phosphate pure substance that it contains is 164kg, and the quality of the magnesium formiate pure substance that it contains is 171kg.
Embodiment 3:
A kind of method for preparing tetramethylolmethane coproduction formic acid and sodium phosphate, 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 816kg, 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; The quality of the tetramethylolmethane pure substance that it contains is 57.12kg;
Step C: the above-mentioned sodium formiate crystal that obtains is water-soluble, be reaction in 6: 0.8 with the ratio of the molar content of the pure substance of sodium formiate and trimagnesium phosphate then, produce magnesium formiate and sodium phosphate, after filtration with trimagnesium phosphate solution, remove a spot of filter residue, obtain containing the filtrate three of magnesium formiate and sodium phosphate;
Step D: filtrate three is the sodium phosphate saturated solution through underpressure distillation, is cooled to 0 ℃, and at this moment, the saturation ratio of sodium phosphate is 4.5g, the saturation ratio of magnesium formiate is 14g, and therefore, the sodium phosphate crystallization is separated out, and magnesium formiate separates still in solution after filtration, obtains sodium phosphate crystal and filtrate four; Filtrate four further underpressure distillation are the magnesium formiate supersaturated solution, are cooled to 0 ℃, and at this moment, the magnesium formiate mass crystallization is separated out, and obtains the magnesium formiate crystal; Sodium phosphate crystal and magnesium formiate crystal advance washing, dry and pulverizing respectively, thereby obtain sodium phosphate product and magnesium formiate product respectively, and the quality of the sodium phosphate pure substance that it contains is 131.2kg, and the quality of the magnesium formiate pure substance that it contains is 136.8kg.
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 magnesium formiate and sodium phosphate 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, be 6 with the ratio of the molar content of the pure substance of sodium formiate and trimagnesium phosphate then with trimagnesium phosphate solution: the 0.8-1.2 reaction, produce magnesium formiate and sodium phosphate, after filtration, remove a spot of filter residue, obtain containing the filtrate three of magnesium formiate and sodium phosphate;
Step D: filtrate three is the sodium phosphate saturated solution through underpressure distillation, is cooled to 0 ℃, and at this moment, the saturation ratio of sodium phosphate is 4.5g, the saturation ratio of magnesium formiate is 14g, and therefore, the sodium phosphate crystallization is separated out, and magnesium formiate separates still in solution after filtration, obtains sodium phosphate crystal and filtrate four; Filtrate four further underpressure distillation are the magnesium formiate supersaturated solution, are cooled to 0 ℃, and at this moment, the magnesium formiate mass crystallization is separated out, and obtains the magnesium formiate crystal; Sodium phosphate crystal and magnesium formiate crystal advance washing, dry and pulverizing respectively, thereby obtain sodium phosphate product and magnesium formiate product respectively.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106112835A CN102115403A (en) | 2010-12-29 | 2010-12-29 | Method for preparing pentaerythritol and co-producing magnesium formate and sodium phosphate |
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|---|---|---|---|
| CN2010106112835A CN102115403A (en) | 2010-12-29 | 2010-12-29 | Method for preparing pentaerythritol and co-producing magnesium formate and sodium phosphate |
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| CN102115403A true CN102115403A (en) | 2011-07-06 |
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| CN2010106112835A Pending CN102115403A (en) | 2010-12-29 | 2010-12-29 | Method for preparing pentaerythritol and co-producing magnesium formate and sodium phosphate |
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Application publication date: 20110706 |