CN102491958A - Production process using chloroacetic acid tail gas to produce epoxy chloropropane - Google Patents
Production process using chloroacetic acid tail gas to produce epoxy chloropropane Download PDFInfo
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- CN102491958A CN102491958A CN2011103583408A CN201110358340A CN102491958A CN 102491958 A CN102491958 A CN 102491958A CN 2011103583408 A CN2011103583408 A CN 2011103583408A CN 201110358340 A CN201110358340 A CN 201110358340A CN 102491958 A CN102491958 A CN 102491958A
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Abstract
The invention provides a production process using chloroacetic acid tail gas to produce epoxy chloropropane. The production process comprises the following process flows: (1), adding glycerine and chloroactic acid mother liquor (5-8% of the glycerine by weight) to a chlorination reaction kettle; (2), mixing the chlorinated liquid of the dichloropropanol with 9-12% of lime emulsion, and then putting the mixture to a reaction tower to perform steam distillation under the pressure of (-)0.04MPa to (-)0.06MPa; (3), removing the moisture of crude epoxy chloropropane generated by the reaction in a pressure-reducing distillation manner, and putting the dehydrated epoxy chloropropane to a rectifying tower to perform rectification under vacuum, and acquiring the product epoxy chloropropane on the top of the rectifying tower. The chloroacetic acid tail gas and the glycerol react, so that the energy is saved, and the investment is a little; the cost advantages are remarkable, the operation conditions of the proposal are gentle, safe and reliable without pollution waste steam; moreover, composite catalyst is adopted in the reaction, and the dear catalyst is not needed.
Description
Technical field
The invention belongs to chemical field, relate in particular to a kind of production technique of utilizing Mono Chloro Acetic Acid tail gas to produce epoxy chloropropane.
Background technology
Epoxy chloropropane is a kind of important Organic Chemicals and fine chemical product; It is strong to be with it that epoxy resin that raw material makes has cohesiveness, characteristics such as resistant to chemical media burn into shrinking percentage is low, chemicalstability good, excellent in cushion effect and dielectric properties excellence.Industrialized epoxy chloropropane production method has three kinds of propylene high-temperature chlorination based on petroleum, propylene acetate method and glycerine methods, and the overwhelming majority is the propylene route.The propylene high-temperature chlorination is that the classical way of producing epoxy chloropropane is gone up in industry, and main raw material is propylene, chlorine and lime, and its technological process mainly comprises: propylene high-temperature chlorination system propenyl chloride; Propenyl chloride hypochlorination synthesizing dichloropropanol (DCH); 3 reaction members of dichlorohydrine saponification synthesizing epoxy chloropropane.The characteristics of propylene high-temperature chlorination are that production process is flexible, technical maturity, and stable operation, shortcoming is that the equipment corrosion that causes of raw material chlorine is serious, the material of purified propylene and reactor drum is required high, and energy consumption is big, and the chlorine consumption is high, and by product is many, and product yield is low; Production process produces a large amount of waste water that contains calcium chloride and organic chloride; Processing costs is high; Coke cleaning period is short, produces required main raw material propylene in addition and derives from oil, belongs to non-renewable raw material; Under the more and more nervous situation of the present whole world energy, there is very big uncertainty in its raw material supply.
Summary of the invention
The present invention is in order to address the above problem, and a kind of production technique of utilizing Mono Chloro Acetic Acid tail gas to produce epoxy chloropropane is provided.
Technical scheme of the present invention is achieved in that the production technique of utilizing Mono Chloro Acetic Acid tail gas to produce epoxy chloropropane, comprises following technical process:
(1), glycerine and mother liquor of chloroacetic acid (pressing the 5%-8% of glycerine weight) are added in the chlorination reaction still; Be warming up to 30-50 ℃; Promptly begin to feed Mono Chloro Acetic Acid tail gas, keep temperature of reaction, keep reaction after 15-18 hour at 85-95 ℃; Stop to feed Mono Chloro Acetic Acid tail gas after the chemical examination dichloropropanol content reaches 84-86%, reaction stops;
(2), the chlorated liquid with above-mentioned dichlorohydrine gets into reaction tower after the 9-12% lime slurry mixes; Under pressure-0.04--0.06MPa, carry out wet distillation; The epoxy chloropropane that generates is taken out of; PH value through waste liquid at the bottom of the adjusting milk of lime add-on adjusting tower is 10-11, and the content of the thick epoxy chloropropane that obtains is at 88-92%;
(3), will react the thick epoxy chloropropane that generates and remove moisture wherein through the mode of underpressure distillation; Pressure is-0.08--0.11MPa; Discharging when moisture content is lower than 0.01%-0.015%; Get into rectifying tower and carry out rectification under vacuum, pressure is-0.08--0.11MPa to obtain the finished product epoxy chloropropane at the rectifying tower cat head;
(4), the epoxy chloropropane of the 3-7% that contains in the rectifying tower bottoms gets into regenerating column; Mode through underpressure distillation steams it; Pressure is-0.08--0.11MPa, and overhead condensation liquid comes back to the recycle of thick epoxy chloropropane storage tank, and high boiling material returns reaction tower secondary response again at the bottom of the tower.
The invention has the beneficial effects as follows: the present invention adopts Mono Chloro Acetic Acid tail gas and glycerine reaction, need not use the hydrochloric acid of chlorine, hypochlorous acid and traditional glycerine method of propylene high-temperature chlorination, belongs to resource and reclaims comprehensive utilization, has greatly saved the energy; Glycerine derives from biological raw material in addition, belongs to renewable energy source, process method environmental protection and save energy, and sustainability is strong, also has bigger advantage than the raw material propylene of propylene high-temperature chlorination; Invest little, be the propylene method 1/4th in addition lower, finished product is than propylene method cost low 1000-3000 per ton unit; Cost advantage is obvious, and the scheme operational condition relaxes, and is safe and reliable; Pollution-free waste vapour produces, and a spot of alkaline water of generation is used for heat power plant's desulfurizer desulfurization, and no waste water effluxes; Composite catalyst is adopted in reaction, does not need expensive catalysts.
Embodiment
In order to understand better and to implement, specify the present invention below and utilize Mono Chloro Acetic Acid tail gas to produce the production technique of epoxy chloropropane: utilize Mono Chloro Acetic Acid tail gas to produce the production technique of epoxy chloropropane, comprise following technical process:
(1), glycerine and mother liquor of chloroacetic acid (press glycerine weight 6%) are added in the chlorination reaction still; Be warming up to 40 ℃; Promptly begin to feed Mono Chloro Acetic Acid tail gas, keep temperature of reaction, keep reaction after 17 hours at 90 ℃; Stop to feed Mono Chloro Acetic Acid tail gas after the chemical examination dichloropropanol content reaches 85%, reaction stops;
(2), the chlorated liquid with above-mentioned dichlorohydrine gets into reaction tower after 10% lime slurry mixes; Under pressure-0.05MPa, carry out wet distillation; The epoxy chloropropane that generates is taken out of; PH value through waste liquid at the bottom of the adjusting milk of lime add-on adjusting tower is 10-11, and the content of the thick epoxy chloropropane that obtains is about 90%;
(3), will react the thick epoxy chloropropane that generates and remove moisture wherein through the mode of underpressure distillation; Pressure is-0.09MPa that discharging when moisture content is lower than 0.01% gets into rectifying tower and carries out rectification under vacuum; Pressure is-0.09MPa to obtain the finished product epoxy chloropropane at the rectifying tower cat head;
(4), the epoxy chloropropane of the 3-7% that contains in the rectifying tower bottoms gets into regenerating column; Mode through underpressure distillation steams it; Pressure is-0.09MPa, and overhead condensation liquid comes back to the recycle of thick epoxy chloropropane storage tank, and high boiling material returns reaction tower secondary response again at the bottom of the tower.
Claims (1)
1. utilize Mono Chloro Acetic Acid tail gas to produce the production technique of epoxy chloropropane, it is characterized in that comprising following technical process:
(1), glycerine and mother liquor of chloroacetic acid (pressing the 5%-8% of glycerine weight) are added in the chlorination reaction still; Be warming up to 30-50 ℃; Promptly begin to feed Mono Chloro Acetic Acid tail gas, keep temperature of reaction, keep reaction after 15-18 hour at 85-95 ℃; Stop to feed Mono Chloro Acetic Acid tail gas after the chemical examination dichloropropanol content reaches 84-86%, reaction stops;
(2), the chlorated liquid with above-mentioned dichlorohydrine gets into reaction tower after the 9-12% lime slurry mixes; Under pressure-0.04--0.06MPa, carry out wet distillation; The epoxy chloropropane that generates is taken out of; PH value through waste liquid at the bottom of the adjusting milk of lime add-on adjusting tower is 10-11, and the content of the thick epoxy chloropropane that obtains is at 88-92%;
(3), will react the thick epoxy chloropropane that generates and remove moisture wherein through the mode of underpressure distillation; Pressure is-0.08--0.11MPa; Discharging when moisture content is lower than 0.01%-0.015%; Get into rectifying tower and carry out rectification under vacuum, pressure is-0.08--0.11MPa to obtain the finished product epoxy chloropropane at the rectifying tower cat head;
(4), the epoxy chloropropane of the 3-7% that contains in the rectifying tower bottoms gets into regenerating column; Mode through underpressure distillation steams it; Pressure is-0.08--0.11MPa, and overhead condensation liquid comes back to the recycle of thick epoxy chloropropane storage tank, and high boiling material returns reaction tower secondary response again at the bottom of the tower.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110358340.8A CN102491958B (en) | 2011-11-14 | 2011-11-14 | Production process using chloroacetic acid tail gas to produce epoxy chloropropane |
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| CN201110358340.8A CN102491958B (en) | 2011-11-14 | 2011-11-14 | Production process using chloroacetic acid tail gas to produce epoxy chloropropane |
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| CN102491958A true CN102491958A (en) | 2012-06-13 |
| CN102491958B CN102491958B (en) | 2014-04-09 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1063540A (en) * | 1965-03-31 | 1967-03-30 | Beck Koller & Co England Ltd | A process for the production of solid epoxide compounds containing aromatic nuclei |
| CN1882522A (en) * | 2003-11-20 | 2006-12-20 | 索尔维公司 | Process for producing dichloropropanol from glycerol, the glycerol coming eventually from the conversion of animal fats in the manufacture of biodiesel |
| CN101157670A (en) * | 2007-11-13 | 2008-04-09 | 武汉理工大学 | Method for synthesizing epichlorohydrin |
| CN101337950A (en) * | 2008-07-30 | 2009-01-07 | 江苏工业学院 | Method for continuously preparing epichlorohydrin by glycerine reaction fractional distillation |
| CN101712661A (en) * | 2009-12-01 | 2010-05-26 | 宁波东港电化有限责任公司 | Method for producing epoxy chloropropane |
-
2011
- 2011-11-14 CN CN201110358340.8A patent/CN102491958B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1063540A (en) * | 1965-03-31 | 1967-03-30 | Beck Koller & Co England Ltd | A process for the production of solid epoxide compounds containing aromatic nuclei |
| CN1882522A (en) * | 2003-11-20 | 2006-12-20 | 索尔维公司 | Process for producing dichloropropanol from glycerol, the glycerol coming eventually from the conversion of animal fats in the manufacture of biodiesel |
| CN101157670A (en) * | 2007-11-13 | 2008-04-09 | 武汉理工大学 | Method for synthesizing epichlorohydrin |
| CN101337950A (en) * | 2008-07-30 | 2009-01-07 | 江苏工业学院 | Method for continuously preparing epichlorohydrin by glycerine reaction fractional distillation |
| CN101712661A (en) * | 2009-12-01 | 2010-05-26 | 宁波东港电化有限责任公司 | Method for producing epoxy chloropropane |
Non-Patent Citations (2)
| Title |
|---|
| GBZA BRAUN: "THE REACTION OF DIBROMOBARBITURIC ACID WITH AMINES", 《J.AM.CHEM.SOC.》, vol. 54, no. 3, 31 March 1932 (1932-03-31), pages 1248 - 1250 * |
| 王星，等: "环氧氯丙烷生产方法综述", 《广东科技》, no. 6, 31 March 2011 (2011-03-31), pages 34 * |
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| CN102491958B (en) | 2014-04-09 |
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Address after: 264117 beijucheng, Dayao Town, Muping District, Yantai City, Shandong Province Patentee after: Yantai East Thermal Power Co.,Ltd. Address before: 264100 Qinshui Korea Industrial Park, Dayao Town, Mouping District, Yantai City, Shandong Province Patentee before: YANTAI HUMON CHEMICAL Co.,Ltd. |