CN102815726A - Method for purifying by-product sodium chloride in dibenzoyl methane production - Google Patents
Method for purifying by-product sodium chloride in dibenzoyl methane production Download PDFInfo
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- CN102815726A CN102815726A CN2012103190051A CN201210319005A CN102815726A CN 102815726 A CN102815726 A CN 102815726A CN 2012103190051 A CN2012103190051 A CN 2012103190051A CN 201210319005 A CN201210319005 A CN 201210319005A CN 102815726 A CN102815726 A CN 102815726A
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- product sodium
- chlor
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- diphenylpropane
- dione
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Abstract
The invention relates to a method for purifying by-product sodium chloride in dibenzoyl methane production. The method includes steps of, step one, using the by-product sodium chloride in the dibenzoyl methane production as a raw material, and calcining the by-product sodium chloride in a tunnel kiln at the temperature of 450-500 DEG C for 20-30 minutes; step two, placing solids obtained from the calcination into water for dissolving to obtain a solution, keeping the temperature of the solution to be 60-80 DEG C, standing the solution until calcined residues in the solution are precipitated and black particles float on the solution surface, separating lower layer precipitate and the black particles floating on the solution surface, and taking a clear liquor; step three, concentrating and steaming the clear liquor, and then performing cooling and crystallizing; and step four, performing centrifugal filtration to obtain crystal particles, and drying the crystal particles to obtain the finished sodium chloride.
Description
Technical field
The present invention relates to the method for purification of by product in a kind of Chemicals production, particularly relate to the method for purification of by product sodium-chlor in a kind of diphenylpropane-1,3-dione(DPPO) production.
Background technology
Diphenylpropane-1,3-dione(DPPO) has the beta-diketon structure, is that a kind of important thermoplastics is used up, thermo-stabilizer, and product is nonpoisonous and tasteless, is widely used in PVC plastics and the ABS resin.Diphenylpropane-1,3-dione(DPPO) has the absorptivity and the lower transsmissivity of broad to ultraviolet ray; Benzophenone that UV absorbing properties is superior to using always and benzotriazole category UV light absorber; And have good thermostability, chemicalstability and light stability, nonpoisonous and tasteless, do not pollute goods.
Diphenylpropane-1,3-dione(DPPO) synthetic operational path is a raw material for adopting oil of Niobe and methyl phenyl ketone, is catalyzer with ethanol/sodium ethylate, is that solvent carries out the synthetic preparation of claisen ketone ester condensation method with YLENE.Along with the increase of production scale, a large amount of sodium-chlor by products of association in process of production.Because this reaction is in xylene solvent, to carry out; Therefore by product solid particle of sodium chloride surface adhesion has a certain amount of YLENE and diphenylpropane-1,3-dione(DPPO); Smell is heavy, and the sodium chloride by product that contains YLENE and diphenylpropane-1,3-dione(DPPO) is contaminate environment not only, also wastes the sodium chloride resource.
Summary of the invention
The technical problem that the present invention will solve provides the method for purification of by product sodium-chlor in a kind of diphenylpropane-1,3-dione(DPPO) production; Sodium-chlor after the purification can reach one-level Industrial Salt national standard; Realized the recycling of by product, and this treating processes can not form secondary pollution.
The method of purification of by product sodium-chlor during a kind of diphenylpropane-1,3-dione(DPPO) is produced may further comprise the steps:
(1) the by product sodium-chlor in the diphenylpropane-1,3-dione(DPPO) production is calcined 20-30min as raw material under 450-500 ℃ of temperature in tunnel; By product solid particle of sodium chloride surface adhesion has YLENE and diphenylpropane-1,3-dione(DPPO); Solid is light grey and is mixed with a small amount of black particle after calcining; Staple after detecting calcining except sodium-chlor is the resistates after the diphenylpropane-1,3-dione(DPPO) calcining; This resistates is not dissolved in water, and black particle is the carbon black particle that the organism calcining produces; The size of treatment capacity does not receive the restriction of calcination condition calmly according to the processing power of tunnel.
(2) solid that will calcine gained places the water dissolving to obtain solution; Keep solution temperature at 60-80 ℃ and leave standstill; Deposition takes place resistates in the solution after the calcining also has black particle to float on liquid level, separates the lower sediment thing and floats on the black particle of liquid level, gets clear liquor; Resistates after the resistates after the check calcining is mainly the diphenylpropane-1,3-dione(DPPO) calcining; To calcine the gained solid places water to dissolve; Be to have nothing to do for the concentration of the resistates after water-soluble sodium-chlor and the calcining of water-fast diphenylpropane-1,3-dione(DPPO) and black particle being separated and dissolve gained solution;
(3) concentration and evaporation clear liquor, cooling, crystallization then; Concentration and evaporation and cooling, crystallization are the usual termss that adopts sodium-chlor to purify;
(4) centrifuging obtains crystal grain, the dry finished product sodium-chlor that gets.
The method of purification of by product sodium-chlor during diphenylpropane-1,3-dione(DPPO) of the present invention is produced, wherein said container are the potter's clay preparations.This container can not be used metal material, avoids in calcination process, having metals ion to get into.
The method of purification of by product sodium-chlor during diphenylpropane-1,3-dione(DPPO) of the present invention is produced, wherein said concentration and evaporation clear liquor is in falling film evaporator, to carry out.
The method of purification of by product sodium-chlor during diphenylpropane-1,3-dione(DPPO) of the present invention is produced, the liquid that wherein said centrifuging obtains is used to dissolve the next batch raw material, recycles.
The method of purification of by product sodium-chlor is effectively removed the organism of inorganic salt sodium-chlor surface adhesion with calcination method in the diphenylpropane-1,3-dione(DPPO) production of the present invention, passes through dissolving, deposition, condensing crystal, centrifuging and drying again, makes high purity chlorination sodium.Present method has not only solved the environmental pollution of by-product salt, and has made full use of resource, and the industrial by-product salt after the purification reaches country-level Industrial Salt standard; The present invention in treating processes, have only the centrifuging step have outside draining, but this mother liquor is to recycle, so non-wastewater discharge; Do not form secondary pollution, and the treating processes cost is low, energy expenditure mainly comprises two portions in this method: the first is at calcination stage; The coal consumption amount according to 1000 yuan/ton of coals, approximately needs 20-25 unit about 20-25kg/ ton raw material; Catabiotic second section is concentrating of mother liquor, and this concentrating part only is to obtain supersaturated solution through evaporation section moisture, and its energy consumption cost also is approximately 20-25 unit/ton; Comprehensive above-mentioned two portions energy consumption is handled raw material basic pay per ton and is about 40-50 unit/ton.
Embodiment
Embodiment 1
(1) get by product sodium-chlor in the production of 30g diphenylpropane-1,3-dione(DPPO) and pack in the potter's clay container, under 480 ℃ temperature, in tunnel, calcine 25min, solid is light gray and is mixed with a small amount of black particle through the calcining back;
(2) solid that will calcine gained places the water dissolving to obtain solution; Calculate water consumption according to dissolving 35g sodium-chlor in every 100g water; Solution keeps fluid temperature at 70 ℃ with hot water or steam heating, leaves standstill 1h and makes resistates deposition and black particle after diphenylpropane-1,3-dione(DPPO) is calcined float on liquid level; Separate the lower sediment thing and float on the black particle of liquid level, get clear liquor;
(3) concentration and evaporation to thick porridge shape in falling film evaporator is reduced to room temperature, crystallization then;
(4) centrifuging obtains crystal grain, and crystal grain is dry on salt drier, and gained sodium-chlor reaches one-level Industrial Salt national standard.
Embodiment 2
(1) get by product sodium-chlor in the production of 100g diphenylpropane-1,3-dione(DPPO) and pack in the potter's clay container, under 500 ℃ temperature, in tunnel, calcine 30min, solid is light gray and is mixed with a small amount of black particle through the calcining back;
(2) solid that will calcine gained places the water dissolving to obtain solution; Calculate water consumption according to dissolving 35g sodium-chlor in every 100g water; Solution keeps fluid temperature at 80 ℃ with hot water or steam heating, leaves standstill 1h and makes resistates deposition and black particle after diphenylpropane-1,3-dione(DPPO) is calcined float on liquid level; Separate the lower sediment thing and float on the black particle of liquid level, get clear liquor;
(3) concentration and evaporation to thick porridge shape in falling film evaporator is reduced to room temperature, crystallization then;
(4) centrifuging obtains crystal grain, and crystal grain is dry on salt drier, and gained sodium-chlor reaches one-level Industrial Salt national standard.
Embodiment 3
(1) get by product sodium-chlor in the production of 200g diphenylpropane-1,3-dione(DPPO) and pack in the potter's clay container, under 450 ℃ temperature, in tunnel, calcine 30min, solid is light gray and is mixed with a small amount of black particle through the calcining back;
(2) solid that will calcine gained places the water dissolving to obtain solution; Calculate water consumption according to dissolving 35g sodium-chlor in every 100g water; Solution keeps fluid temperature at 75 ℃ with hot water or steam heating, leaves standstill 1h and makes resistates deposition and black particle after diphenylpropane-1,3-dione(DPPO) is calcined float on liquid level; Separate the lower sediment thing and float on the black particle of liquid level, get clear liquor;
(3) concentration and evaporation to thick porridge shape in falling film evaporator is reduced to room temperature, crystallization then;
(4) centrifuging obtains crystal grain, and crystal grain is dry on salt drier, and gained sodium-chlor reaches one-level Industrial Salt national standard.
Above-described embodiment describes preferred implementation of the present invention; Be not that scope of the present invention is limited; Design under the prerequisite of spirit not breaking away from the present invention; Various distortion and improvement that those of ordinary skills make technical scheme of the present invention all should fall in the definite protection domain of claims of the present invention.
Claims (4)
1. the method for purification of by product sodium-chlor during a diphenylpropane-1,3-dione(DPPO) is produced is characterized in that may further comprise the steps:
(1) the by product sodium-chlor in the diphenylpropane-1,3-dione(DPPO) production is calcined 20-30min as raw material under 450-500 ℃ of temperature in tunnel;
(2) solid that will calcine gained places the water dissolving to obtain solution; Keep solution temperature at 60-80 ℃ and leave standstill; Deposition takes place resistates in the solution after the calcining also has black particle to float on liquid level, separates the lower sediment thing and floats on the black particle of liquid level, gets clear liquor;
(3) concentration and evaporation clear liquor, cooling, crystallization then;
(4) centrifuging obtains crystal grain, the dry finished product sodium-chlor that gets.
2. the method for purification of by product sodium-chlor during diphenylpropane-1,3-dione(DPPO) according to claim 1 is produced is characterized in that: said container is the potter's clay preparation.
3. the method for purification of by product sodium-chlor during diphenylpropane-1,3-dione(DPPO) according to claim 2 is produced, it is characterized in that: said concentration and evaporation clear liquor is in falling film evaporator, to carry out.
4. the method for purification of by product sodium-chlor during diphenylpropane-1,3-dione(DPPO) according to claim 3 is produced, it is characterized in that: the liquid that said centrifuging obtains is used to dissolve the next batch raw material, recycles.
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| CN2012103190051A CN102815726A (en) | 2012-08-31 | 2012-08-31 | Method for purifying by-product sodium chloride in dibenzoyl methane production |
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| CN2012103190051A CN102815726A (en) | 2012-08-31 | 2012-08-31 | Method for purifying by-product sodium chloride in dibenzoyl methane production |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104085905A (en) * | 2014-07-18 | 2014-10-08 | 安徽佳先功能助剂股份有限公司 | Method for purifying sodium chloride as by-product in production of dibenzoyl methane |
| CN111574713A (en) * | 2020-06-16 | 2020-08-25 | 四川明道和化学新材料有限公司 | Method for recovering polyphenylene sulfide byproduct salt |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1034907A (en) * | 1988-07-09 | 1989-08-23 | 湖北省烟草公司建始县公司 | With the cigarette muscle is the method for raw material production sylvite |
| CN101348266A (en) * | 2008-09-05 | 2009-01-21 | 江苏扬农化工股份有限公司 | Comprehensive processing method of N-phosphonomethyliminodiacelic acid mother liquor |
-
2012
- 2012-08-31 CN CN2012103190051A patent/CN102815726A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1034907A (en) * | 1988-07-09 | 1989-08-23 | 湖北省烟草公司建始县公司 | With the cigarette muscle is the method for raw material production sylvite |
| CN101348266A (en) * | 2008-09-05 | 2009-01-21 | 江苏扬农化工股份有限公司 | Comprehensive processing method of N-phosphonomethyliminodiacelic acid mother liquor |
Non-Patent Citations (3)
| Title |
|---|
| 李运涛: "《无机及分析化学实验》", 31 August 2011 * |
| 梅光泉等: "二苯甲酰甲烷的合成与热稳定性研究", 《宝鸡文理学院学报（自然科学版）》 * |
| 王广生: "《石油化工原料与产品安全手册》", 31 August 2010, 中国石化出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104085905A (en) * | 2014-07-18 | 2014-10-08 | 安徽佳先功能助剂股份有限公司 | Method for purifying sodium chloride as by-product in production of dibenzoyl methane |
| CN111574713A (en) * | 2020-06-16 | 2020-08-25 | 四川明道和化学新材料有限公司 | Method for recovering polyphenylene sulfide byproduct salt |
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Application publication date: 20121212 |