CN102115369A - Method for preparing pentaerythritol, calcium formate and sodium hydroxide by using waste liquid from preparation of pentaerythritol - Google Patents
Method for preparing pentaerythritol, calcium formate and sodium hydroxide by using waste liquid from preparation of pentaerythritol Download PDFInfo
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- CN102115369A CN102115369A CN2010106110007A CN201010611000A CN102115369A CN 102115369 A CN102115369 A CN 102115369A CN 2010106110007 A CN2010106110007 A CN 2010106110007A CN 201010611000 A CN201010611000 A CN 201010611000A CN 102115369 A CN102115369 A CN 102115369A
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Abstract
The invention relates to the technical field of treatment and comprehensive utilization of waste liquid from the preparation of pentaerythritol, in particular to a method for producing pentaerythritol, calcium formate and sodium hydroxide by using waste liquid from the preparation of pentaerythritol. The method mainly comprises: distilling waste liquid from the preparation of pentaerythritol under reduced pressure, and treating the obtained pentaerythritol to obtain a pentaerythritol product; and reacting sodium formate with calcium hydroxide, filtering, further treating the filter cake to obtain a calcium formate product, and distilling the filtrate again to obtain sodium hydroxide. In the invention, the waste liquid can be removed completely, so the pollution of waste residue to the environment is reduced; valuable calcium formate and sodium hydroxide products are produced; and thus, obvious social and economic benefit is created. The process and production equipment are simple, and the method is a practical treatment and utilization method.
Description
Technical field
The present invention relates to prepare the improvement and the comprehensive utilization technique field of the waste liquid that tetramethylolmethane produces, the method that particularly a kind of waste liquid that produces with the preparation tetramethylolmethane is produced tetramethylolmethane coproduction calcium formiate and sodium hydroxide.
Technical background
Tetramethylolmethane is a kind of organic intermediate of having many uses, often be used to coatings industry, it is the raw material of alkydpaints, hardness, glossiness and the weather resistance of paint film are improved, but also can make 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.
The low temperature condensation method is normally adopted in the preparation of tetramethylolmethane, is to be raw material with formaldehyde and acetaldehyde, and condensation makes in the presence of basic catalyst.Be exactly specifically: earlier 37% formaldehyde and sodium hydroxide and acetaldehyde are mixed, and under condition of stirring, slowly be warming up to 25 ℃～32 ℃ and heat, keep this temperature and stirred 6～7 hours with steam; Add with the equimolar sulfuric acid of sodium hydroxide again and neutralize; Last filtrate vapourisation under reduced pressure concentrates, crystallization, filtration and drying make finished product.
In the whole process of preparation, can produce a large amount of waste liquids when filtering and washing; And contain sodium formiate 25%～40%, tetramethylolmethane 6%～8%, other organic substances 15% in these waste liquids.Through statistics, the mother liquor quantity discharged of producing tetramethylolmethane product per ton is 2～3 tons; The waste liquid that the preparation tetramethylolmethane is produced normally simply precipitates and emits after removal of impurities is handled at present, so not only environment is had certain pollution, and slatterns a lot of valuable materials in the waste liquid; The waste liquid that preparation tetramethylolmethane at present also of no use produces is produced the relevant report of the method for tetramethylolmethane coproduction calcium formiate and sodium hydroxide.
Summary of the invention
The invention provides the side that a kind of waste liquid that produces with the preparation tetramethylolmethane is produced tetramethylolmethane coproduction calcium formiate and sodium hydroxide, this method not only technology is simple, and can also make multiple value product when can effectively handle waste residue.
To achieve the above object, technical scheme of the present invention is:
The method that a kind of waste liquid that produces with the preparation tetramethylolmethane is produced tetramethylolmethane coproduction calcium formiate and sodium hydroxide comprises being prepared as follows step:
Steps A, elder generation send into the waste liquid that is produced in the low temperature condensation method production tetramethylolmethane process in the first underpressure distillation device and carry out underpressure distillation; When reaching capacity solution, eject, again with first water cooler cool off, crystallization; Crystals of pentaerythritol and sodium formiate crystal have successively been obtained;
Step B, gained crystals of pentaerythritol in the steps A is carried out being packaged to be the crystals of pentaerythritol product after washing and spin-drying machine, moisture eliminator, the pulverizing with first washing and spin-drying machine, first moisture eliminator, first pulverizer successively;
Step C, be dissolved in according to weight ratio 1: 3 gained sodium formiate crystal in the steps A water-soluble;
Step D, gained sodium formate solution and aqua calcis among the step C put in the reactor with pure mass ratio 1: 0.27～0.67 react, generate calcium formiate precipitation and sodium hydroxide mixed solution I;
Step e, gained mixed solution I among the step D is filtered with strainer;
Step F, after carrying out washing and spin-drying machine, moisture eliminator, pulverizing successively, second washing and spin-drying machine, second moisture eliminator, second pulverizer be packaged to be the calcium formiate product successively with filtering the gained filter cake in the step e;
Step G, in the second underpressure distillation device, carry out underpressure distillation with filtering gained filtrate in the step e; When reaching capacity solution, eject, cool off successively, be packaged to be the sodium hydroxide crystal product behind the washing and spin-drying machine, moisture eliminator, pulverizing with second water cooler, the 3rd washing and spin-drying machine, the 3rd moisture eliminator, the 3rd pulverizer.
Reaction principle of the present invention is:
2CHO
2Na+Ca(OH)
2＝＝＝＝(CHO
2)
2Ca+2NaOH
The present invention mainly is that the waste liquid that will prepare the tetramethylolmethane generation earlier carries out underpressure distillation, and then the tetramethylolmethane that obtains handled obtain the tetramethylolmethane product, sodium formiate and calcium hydroxide are reacted after-filtration, filter cake is further handled and is obtained the calcium formiate product, and filtrate is distilled again and obtained sodium hydroxide; The present invention can as clean as a pennyly gulp down waste liquid, alleviates the pollution of waste residue to environment; Can make valuable calcium formiate and sodium hydroxide product again, not only have remarkable social benefit and economic benefit, and technology and production unit are simple, be a kind of relatively actual processing and utilize method.
Concrete embodiment
Embodiment 1
The method that a kind of waste liquid that produces with the preparation tetramethylolmethane is produced tetramethylolmethane coproduction calcium formiate and sodium hydroxide comprises being prepared as follows step:
Steps A, elder generation produce the waste liquid (if calculate according to 1000Kg, then wherein, contain sodium formiate 300Kg, contain tetramethylolmethane 80Kg) that is produced in the tetramethylolmethane process with the low temperature condensation method and send in the first underpressure distillation device and carry out underpressure distillation; When reaching capacity solution, eject, again with first water cooler cool off, crystallization; Crystals of pentaerythritol and sodium formiate crystal have successively been obtained;
Step B, gained crystals of pentaerythritol in the steps A is carried out being packaged to be 80Kg crystals of pentaerythritol product after washing and spin-drying machine, moisture eliminator, the pulverizing with first washing and spin-drying machine, first moisture eliminator, first pulverizer successively;
Step C, be dissolved in according to weight ratio 1: 3 gained sodium formiate crystal in the steps A water-soluble;
Step D, gained sodium formate solution and aqua calcis among the step C put in reactor with pure mass ratio at 1: 0.27 react, generate calcium formiate precipitation and sodium hydroxide mixed solution I;
Step e, gained mixed solution I among the step D is filtered with strainer;
Step F, after carrying out washing and spin-drying machine, moisture eliminator, pulverizing successively, second washing and spin-drying machine, second moisture eliminator, second pulverizer be packaged to be 142.21Kg calcium formiate product successively with filtering the gained filter cake in the step e;
Step G, in the second underpressure distillation device, carry out underpressure distillation with filtering gained filtrate in the step e; When reaching capacity solution, eject, cool off successively, be packaged to be 87.45Kg sodium hydroxide crystal product behind the washing and spin-drying machine, moisture eliminator, pulverizing with second water cooler, the 3rd washing and spin-drying machine, the 3rd moisture eliminator, the 3rd pulverizer.
Embodiment 2
The method that a kind of waste liquid that produces with the preparation tetramethylolmethane is produced tetramethylolmethane coproduction calcium formiate and sodium hydroxide comprises being prepared as follows step:
Steps A, elder generation produce the waste liquid (if calculate according to 1000Kg, then wherein, contain sodium formiate 300Kg, contain tetramethylolmethane 80Kg) that is produced in the tetramethylolmethane process with the low temperature condensation method and send in the first underpressure distillation device and carry out underpressure distillation; When reaching capacity solution, eject, again with first water cooler cool off, crystallization; Crystals of pentaerythritol and sodium formiate crystal have successively been obtained;
Step B, gained crystals of pentaerythritol in the steps A is carried out being packaged to be 80Kg crystals of pentaerythritol product after washing and spin-drying machine, moisture eliminator, the pulverizing with first washing and spin-drying machine, first moisture eliminator, first pulverizer successively;
Step C, be dissolved in according to weight ratio 1: 3 gained sodium formiate crystal in the steps A water-soluble;
Step D, gained sodium formate solution and aqua calcis among the step C put in reactor with pure mass ratio at 1: 0.47 react, generate calcium formiate precipitation and sodium hydroxide mixed solution I;
Step e, gained mixed solution I among the step D is filtered with strainer;
Step F, after carrying out washing and spin-drying machine, moisture eliminator, pulverizing successively, second washing and spin-drying machine, second moisture eliminator, second pulverizer be packaged to be 247.55Kg calcium formiate product successively with filtering the gained filter cake in the step e;
Step G, in the second underpressure distillation device, carry out underpressure distillation with filtering gained filtrate in the step e; When reaching capacity solution, eject, cool off successively, be packaged to be 152.23Kg sodium hydroxide crystal product behind the washing and spin-drying machine, moisture eliminator, pulverizing with second water cooler, the 3rd washing and spin-drying machine, the 3rd moisture eliminator, the 3rd pulverizer.
Embodiment 3
The method that a kind of waste liquid that produces with the preparation tetramethylolmethane is produced tetramethylolmethane coproduction calcium formiate and sodium hydroxide comprises being prepared as follows step:
Steps A, elder generation produce the waste liquid (if calculate according to 1000Kg, then wherein, contain sodium formiate 300Kg, contain tetramethylolmethane 80Kg) that is produced in the tetramethylolmethane process with the low temperature condensation method and send in the first underpressure distillation device and carry out underpressure distillation; When reaching capacity solution, eject, again with first water cooler cool off, crystallization; Crystals of pentaerythritol and sodium formiate crystal have successively been obtained;
Step B, gained crystals of pentaerythritol in the steps A is carried out being packaged to be 80Kg crystals of pentaerythritol product after washing and spin-drying machine, moisture eliminator, the pulverizing with first washing and spin-drying machine, first moisture eliminator, first pulverizer successively;
Step C, be dissolved in according to weight ratio 1: 3 gained sodium formiate crystal in the steps A water-soluble;
Step D, gained sodium formate solution and aqua calcis among the step C put in reactor with pure mass ratio at 1: 0.67 react, generate calcium formiate precipitation and sodium hydroxide mixed solution I;
Step e, gained mixed solution I among the step D is filtered with strainer;
Step F, after carrying out washing and spin-drying machine, moisture eliminator, pulverizing successively, second washing and spin-drying machine, second moisture eliminator, second pulverizer be packaged to be 253.89Kg calcium formiate product successively with filtering the gained filter cake in the step e;
Step G, in the second underpressure distillation device, carry out underpressure distillation with filtering gained filtrate in the step e; When reaching capacity solution, eject, cool off successively, be packaged to be 217.01Kg sodium hydroxide crystal product behind the washing and spin-drying machine, moisture eliminator, pulverizing with second water cooler, the 3rd washing and spin-drying machine, the 3rd moisture eliminator, the 3rd pulverizer.
The foregoing description is preferred embodiment of the present invention, is not to be used for limiting the scope of the present invention, so all equivalences of being done with described feature of claim of the present invention and principle change or modify, all should be included within the claim scope of the present invention.
Claims (1)
1. the method that the waste liquid that produces with the preparation tetramethylolmethane is produced tetramethylolmethane coproduction calcium formiate and sodium hydroxide is characterized in that, comprises being prepared as follows step:
Steps A, elder generation send into the waste liquid that is produced in the low temperature condensation method production tetramethylolmethane process in the first underpressure distillation device and carry out underpressure distillation; When reaching capacity solution, eject, again with first water cooler cool off, crystallization; Crystals of pentaerythritol and sodium formiate crystal have successively been obtained;
Step B, gained crystals of pentaerythritol in the steps A is carried out being packaged to be the crystals of pentaerythritol product after washing and spin-drying machine, moisture eliminator, the pulverizing with first washing and spin-drying machine, first moisture eliminator, first pulverizer successively;
Step C, be dissolved in according to weight ratio 1: 3 gained sodium formiate crystal in the steps A water-soluble;
Step D, gained sodium formate solution and aqua calcis among the step C put in the reactor with pure mass ratio 1: 0.27～0.67 react, generate calcium formiate precipitation and sodium hydroxide mixed solution I;
Step e, gained mixed solution I among the step D is filtered with strainer;
Step F, after carrying out washing and spin-drying machine, moisture eliminator, pulverizing successively, second washing and spin-drying machine, second moisture eliminator, second pulverizer be packaged to be the calcium formiate product successively with filtering the gained filter cake in the step e;
Step G, in the second underpressure distillation device, carry out underpressure distillation with filtering gained filtrate in the step e; When reaching capacity solution, eject, cool off successively, be packaged to be the sodium hydroxide crystal product behind the washing and spin-drying machine, moisture eliminator, pulverizing with second water cooler, the 3rd washing and spin-drying machine, the 3rd moisture eliminator, the 3rd pulverizer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106110007A CN102115369A (en) | 2010-12-29 | 2010-12-29 | Method for preparing pentaerythritol, calcium formate and sodium hydroxide by using waste liquid from preparation of pentaerythritol |
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|---|---|---|---|
| CN2010106110007A CN102115369A (en) | 2010-12-29 | 2010-12-29 | Method for preparing pentaerythritol, calcium formate and sodium hydroxide by using waste liquid from preparation of pentaerythritol |
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| CN2010106110007A Pending CN102115369A (en) | 2010-12-29 | 2010-12-29 | Method for preparing pentaerythritol, calcium formate and sodium hydroxide by using waste liquid from preparation of pentaerythritol |
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Application publication date: 20110706 |