CN112142690A - Process for producing epichlorohydrin by using chlorinated paraffin and chlorine-containing tail gas glycerin method - Google Patents
Process for producing epichlorohydrin by using chlorinated paraffin and chlorine-containing tail gas glycerin method Download PDFInfo
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- CN112142690A CN112142690A CN202011141703.8A CN202011141703A CN112142690A CN 112142690 A CN112142690 A CN 112142690A CN 202011141703 A CN202011141703 A CN 202011141703A CN 112142690 A CN112142690 A CN 112142690A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D301/00—Preparation of oxiranes
- C07D301/02—Synthesis of the oxirane ring
- C07D301/24—Synthesis of the oxirane ring by splitting off HAL—Y from compounds containing the radical HAL—C—C—OY
- C07D301/26—Y being hydrogen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/24—Chlorides
- C01F11/28—Chlorides by chlorination of alkaline-earth metal compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/24—Chlorides
- C01F11/30—Concentrating; Dehydrating; Preventing the adsorption of moisture or caking
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/24—Chlorides
- C01F11/32—Purification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D301/00—Preparation of oxiranes
- C07D301/32—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D303/00—Compounds containing three-membered rings having one oxygen atom as the only ring hetero atom
- C07D303/02—Compounds containing oxirane rings
- C07D303/08—Compounds containing oxirane rings with hydrocarbon radicals, substituted by halogen atoms, nitro radicals or nitroso radicals
Abstract
The invention discloses a process for producing epichlorohydrin by a glycerin method by using chlorinated paraffin chlorine-containing tail gas, which comprises the steps of chlorinating glycerin by using gaseous hydrogen chloride in a reaction kettle, distilling at least once, and saponifying obtained fractions by using alkali liquor to obtain epichlorohydrin. The method specifically comprises the steps of chlorohydrination of glycerol, primary distillation, saponification reaction, water removal, secondary distillation and the like, the process is simple and controllable, the generation of tar in the production process of epoxy chloropropane is greatly reduced, the color quality of the produced ECH finished product is less than 5, and the quality of the ECH product is greatly improved. In addition, the glycerol chlorination of the invention opens up a new way for utilizing the tail gas generated in the chlorinated paraffin production process to adopt the tail gas containing chlorine generated in the chlorinated paraffin production process. In addition, the invention concentrates the calcium chloride solution obtained by saponification reaction into calcium chloride solid, and makes full use of the value of the production raw material; the invention has important practical and economic values and simultaneously has good ecological and social benefits.
Description
Technical Field
The invention relates to a process for producing epichlorohydrin by a glycerol method by using chlorinated paraffin chlorine-containing tail gas.
Background
Epichlorohydrin (ECH) is an important organic synthetic intermediate, and epoxy resin prepared by using the ECH as a raw material is widely applied to the fields of coatings, adhesives, electronic laminates and the like. In addition, epichlorohydrin can also be used for producing synthetic glycerin, nitroglycerin explosive, glass fiber reinforced plastic, electrical insulation products, surfactants, medicines, pesticides, coatings, ion exchange resins, plasticizers, epichlorohydrin rubber and the like. The fine chemical products are widely applied to the industries of chemical industry, light industry, transportation, medicine, coating, food, electronic and electric appliances and the like. China is the largest production base of epoxy resin in the world, and the consumption proportion of epoxy chloropropane in China is as follows: 85% of epoxy resin, 7% of synthetic glycerol, 2% of epichlorohydrin rubber and 6% of others (including solvents, stabilizers, surfactants, flame retardants, oilfield chemicals, water treatment agents and the like); therefore, the demand of China on the epoxy chloropropane product is great.
At present, the industrial methods for producing epichlorohydrin in the world mainly comprise the following three methods: (1) propylene high-temperature chlorination (referred to as chloropropene method hereinafter) represented by Shell company in America, wherein the intermediate product is 3-chloropropene, and finally epichlorohydrin is prepared. At present, more than 95 percent of epoxy chloropropane in the world is produced by adopting the method (2) an allyl acetate-allyl alcohol method (hereinafter referred to as allyl alcohol method) which is developed and industrialized in the middle of 80 years of Japanese Zhao and electrician, wherein the intermediate product is allyl alcohol. (3) The glycerol method adopts a glycerol method to produce epichlorohydrin, and then adopts a two-step method to produce epoxy resin. The first two of the two take propylene as an upstream raw material, however, the production cost is higher and higher with the continuous increase of the cost of the propylene; and a chloropropene method which is a main production method of epoxy chloropropane. The process needs high-temperature conditions, and production equipment runs at high temperature for a long time, so that potential safety hazards are easily encountered, and more abnormal parking faults are caused.
The glycerol method is researched as early as 40 years ago, but because the glycerol is tense and the consumption of the glycerol method is high, the glycerol method gradually fades out of view. In recent years, with the progress and development of technology, the product quality produced by the developed reagent-grade glycerol method device is far better than that produced by the current industrial-grade device, so that the capacity and the technical bottleneck of the epichlorohydrin do not exist. However, with the continuous expansion of the production of ECH by the national glycerin method, a large number of problems are exposed, for example, a large amount of tar is generated in the reaction process of chlorohydrin, and the amount of tar generated in the process of most enterprises is about 15%, which seriously limits the improvement of product quality and greatly reduces the utilization rate of raw materials; and the produced ECH finished product has high color quality, generally more than 5, and the quality of the product is visually influenced.
Disclosure of Invention
Aiming at the problems, the invention provides a process for producing epichlorohydrin by a glycerin method by using chlorine-containing tail gas of chlorinated paraffin, which prepares ECH by chlorohydrination of glycerin by using chlorine-containing hydrogen chloride, greatly reduces the generation of tar and ensures that the color quality of the produced ECH finished product is less than 5. The specific technical scheme is as follows:
a process for preparing epoxy chloropropane by glycerin method features that the chlorine-contained tail gas of chlorinated paraffin is chlorohydrated by gaseous hydrogen chloride in reactor, and the fraction obtained is saponified by alkali solution to obtain epoxy chloropropane.
The process for producing epichlorohydrin by using chlorinated paraffin chlorine-containing tail gas through the glycerol method specifically comprises the following steps:
1) chlorohydrination of glycerol: carrying out chlorohydrination reaction on glycerol, chlorine-containing tail gas from a paraffin workshop and a prepared catalyst in a chlorohydrination reaction kettle to obtain dichloropropanol;
2) primary distillation: dichloropropanol obtained by glycerol chlorination is distilled by a rectifying tower to obtain dichloropropanol, water and hydrochloric acid;
3) saponification reaction: reacting dichloropropanol, water and hydrochloric acid obtained by primary distillation with a prepared calcium hydroxide aqueous solution in a mixer according to a certain proportion, and then sending the mixture into a saponification tower for saponification reaction to obtain primary epichlorohydrin;
4) dewatering: sending the primary epoxy chloropropane obtained by saponification into a dewatering tower to remove water, and obtaining a semi-finished product of epoxy chloropropane;
5) secondary distillation: and (4) sending the semi-finished product of the epoxy chloropropane obtained after the water removal into the rectifying tower again for secondary distillation to obtain the finished product of the epoxy chloropropane.
As a preferable technical scheme, in the step 1), the concentration of the glycerol is 95%, and the introduced flow rate is 2000 kg/h; the inlet flow of the chlorine-containing tail gas from the paraffin workshop is 2000 kg/h.
In a preferable technical scheme, in the step 1), the dosage of the catalyst composite chlorination catalyst needs to be adjusted at any time according to production load, and generally the weight ratio of the dosage of the catalyst to glycerol is 1: 0.1-0.5.
In a preferable technical scheme, in the step 1), the reaction temperature of glycerol chlorination and chlorohydrination is controlled to be 100-140 ℃.
Preferably, in the step 2), the temperature of the bottom of the primary distillation tower is controlled to be 145-155 ℃.
As a preferable technical scheme, in the step 3), the concentration of the calcium hydroxide aqueous solution used for the saponification reaction is 25%; and (3) carrying out dry distillation on the dichloropropanol, the water and the hydrochloric acid at the flow rate of 4m/h, and mixing the mixture with the calcium hydroxide aqueous solution at the ratio of 1: 1-3, wherein the reaction temperature of the saponification tower is controlled to be 95-105 ℃.
In a preferable technical scheme, in the step 4), the water removal temperature is controlled to be 125-135 ℃.
Preferably, in the step 5), the temperature of the bottom of the secondary distillation tower is controlled to be 135-145 ℃.
The process for producing epichlorohydrin by using chlorinated paraffin chlorine-containing tail gas in a glycerol method also comprises a calcium chloride recovery process, and specifically comprises the following steps: carrying out filter pressing and concentration equipment on the calcium chloride solution generated by the saponification reaction in the step 3) to obtain a calcium chloride solution with the concentration of 40%; concentrating again by climbing film to make its concentration reach 70%; finally, slicing by a slicer, drying and cooling to form calcium chloride solid with qualified quality.
The invention has the beneficial effects that:
in the process, chlorohydrination is carried out on glycerol by using gaseous hydrogen chloride in a reaction kettle, distillation is carried out at least once, and the obtained fraction is saponified by alkali liquor to obtain epoxy chloropropane; the process is simple, the process is controllable, the generation of tar in the production process of epoxy chloropropane is greatly reduced, and the tar amount is only one tenth of that generated in the production of similar products; and the color quality of the ECH finished product produced by the process is less than 5, so that the breakthrough that the color quality of the finished product in the domestic field is less than 5 is realized for the first time, the quality of the ECH product is greatly improved, and the ECH finished product has important practical and economic values. In addition, the gaseous hydrogen chloride for chlorohydrination of the glycerol is chlorine-containing tail gas generated in the production process of chlorinated paraffin, so that a new way for utilizing the tail gas generated in the production of the chlorinated paraffin is developed, a new way is developed for green and environment-friendly production of the chlorinated paraffin, and important ecological and environmental benefits are achieved. In addition, the invention also provides a calcium chloride liquid concentration process obtained by saponification, which makes full use of the value of production raw materials, makes the best use of things, reduces the discharge of waste liquid and waste gas, and further improves the economic and environmental benefits.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments. The embodiment 1 is a process for producing epichlorohydrin by using chlorinated paraffin chlorine-containing tail gas through a glycerol method, and the embodiments 2 to 4 are processes for producing epichlorohydrin by using the process described in the embodiment 1.
Example 1
This example is a process for producing epichlorohydrin by using chlorinated paraffin chlorine-containing tail gas glycerin process, in which glycerin is chlorohydrinated with gaseous hydrogen chloride in a reaction kettle, and at least once distilled, and the obtained fraction is saponified with alkali liquor to obtain epichlorohydrin. The method specifically comprises the following steps:
1) chlorohydrination of glycerol: carrying out chlorohydrination reaction on 95% glycerol, chlorine-containing tail gas from a paraffin production workshop and a prepared catalyst in a chlorination reaction kettle to obtain dichloropropanol. The flow rate of the introduced glycerol is 2000kg/h, and the flow rate of the introduced chlorine-containing tail gas from a paraffin workshop is 2000 kg/h; the catalyst is a composite chlorination catalyst produced by Changzhou good new material science and technology limited company, and the weight ratio of the dosage of the catalyst to the glycerol is 1: 0.1-0.5; the reaction temperature of the chlorohydrination of the glycerol is controlled to be 100-140 ℃.
2) Primary distillation: introducing dichloropropanol obtained by chlorohydrination of glycerol into a rectifying tower for primary distillation, controlling the temperature at the bottom of the rectifying tower to be 145-155 ℃, and carrying out primary distillation to obtain the dichloropropanol, water and hydrochloric acid.
3) Saponification reaction: and (2) carrying out a reaction on dichloropropanol, water and hydrochloric acid obtained by primary distillation at a flow rate of 4m/h and a prepared 25% calcium hydroxide aqueous solution according to a ratio of 1: 1-3 in a mixer, then sending the mixture into a saponification tower for saponification, feeding unreacted materials into the saponification tower in the mixer for subsequent reaction, and controlling the saponification reaction temperature to be 95-105 ℃ to obtain the primary epoxy chloropropane. The calcium chloride solution generated by saponification is concentrated into calcium chloride solution with the concentration of 40 percent by filter pressing and concentration equipment; concentrating again by climbing film to make its concentration reach 70%; finally, slicing by a slicer, drying and cooling to form calcium chloride solid with qualified quality.
4) Dewatering: and (3) sending the primary epoxy chloropropane obtained by saponification into a water removal tower, and controlling the water removal tower to be 125-135 ℃ to remove moisture in the epoxy chloropropane to obtain a semi-finished product of the epoxy chloropropane.
5) Secondary distillation: and (4) sending the semi-finished product of the epoxy chloropropane obtained after the water removal into the rectifying tower again for secondary distillation to obtain the finished product of the epoxy chloropropane.
Example 2
In this embodiment, epichlorohydrin is also produced by using the process described in embodiment 1, specifically as follows:
the glycerol with the concentration of 95 percent reacts with chlorine-containing tail gas from a paraffin workshop and a prepared catalyst with the flow rate of 2000kg/h in a chlorination reaction kettle, and the temperature of the reaction kettle is controlled at 120 ℃. And (3) introducing the dichloropropanol from the reaction kettle into a rectifying tower for primary distillation, controlling the temperature at the bottom of the rectifying tower to be 145 ℃, and collecting the dichloropropanol, water and hydrochloric acid distilled from the top of the tower to enter the next link. Returning the tower bottom high-boiling substances (including glycerol, dichloropropanol and monochloropropaneol) to the chlorination reaction kettle again to continue the reaction. And the gas phase condensate of the chlorination reaction kettle and dichloropropanol, water and hydrochloric acid materials condensed by a condenser at the top of the distillation tower enter the same storage tank together for further use.
Dichloropropanol, water and hydrochloric acid distilled out for the first time enter a mixer at the flow rate of 4m/h and 25% of calcium hydroxide aqueous solution prepared in advance according to the proportion of 1:1.5 for mixing reaction, then the mixture is introduced into a saponification tower for saponification reaction (the unreacted materials in the mixer enter the saponification tower for subsequent reaction), the saponification reaction temperature is controlled at 95 ℃, and primary ECH discharged from the top of the saponification tower is collected. The concentration of the calcium chloride solution from the bottom of the saponification tower is about 15%, and the calcium chloride solution is concentrated into 40% calcium chloride solution through first-effect and second-effect concentration equipment after filter pressing; finally, concentrating again by climbing a film to ensure that the concentration reaches 70 percent; slicing by a slicer, drying, cooling and packaging to obtain qualified calcium chloride solid.
The primary ECH from the top of the saponification tower contains a large amount of water, so that the ECH is obtained by removing the water through a water removal tower, and the temperature of the water removal tower is controlled at 125 ℃. And (3) performing secondary distillation on the ECH in a rectifying tower to obtain a finished product, wherein the tower bottom temperature of the secondary distillation rectifying tower is controlled at 135 ℃. The tar yield in this example was 1% and the resulting finished ECH product had a color quality of 2.8, as tested.
Example 3
In this example, epichlorohydrin was produced by the process described in example 1, specifically as follows:
the glycerol with the concentration of 95 percent reacts with chlorine-containing tail gas from a paraffin workshop and a prepared catalyst with the flow rate of 2000kg/h in a chlorohydrination reaction kettle, and the temperature of the reaction kettle is controlled at 120 ℃. And (3) introducing the dichloropropanol from the reaction kettle into a rectifying tower for primary distillation, controlling the temperature at the bottom of the rectifying tower to be 150 ℃, and collecting the dichloropropanol, water and hydrochloric acid distilled from the top of the tower to enter the next link. Returning the tower bottom high-boiling substances (including glycerol, dichloropropanol and monochloropropaneol) to the chlorination reaction kettle again to continue the reaction. And the gas phase condensate of the chlorination reaction kettle and the material condensed by the condenser at the top of the distillation tower enter the same storage tank together for further use.
Dichloropropanol, water and hydrochloric acid distilled out for the first time enter a mixer at the flow rate of 4m/h and 25% of calcium hydroxide aqueous solution prepared in advance according to the proportion of 1: to react, then the mixture is sent into a saponification tower to carry out saponification, the saponification reaction temperature is controlled at 100 ℃, and primary ECH discharged from the top of the saponification tower is collected. The concentration of the calcium chloride solution from the bottom of the saponification tower is about 15%, and the calcium chloride solution is concentrated into 40% calcium chloride solution through first-effect and second-effect concentration equipment after filter pressing; finally, concentrating again by climbing a film to ensure that the concentration reaches 70 percent; slicing by a slicer, drying, cooling and packaging to obtain qualified calcium chloride solid.
The primary ECH from the top of the saponification tower contains a large amount of water, so that the ECH is obtained by removing the water through a water removal tower, and the temperature of the water removal tower is controlled at 130 ℃. And performing secondary distillation on the ECH in a rectifying tower to obtain a finished product, wherein the tower bottom temperature of the secondary distillation rectifying tower is controlled at 140 ℃. The amount of tar produced in this example was 1.1%; the resulting finished ECH had a color quality of 2.2.
Example 4
In this embodiment, epichlorohydrin is also produced by the process described in embodiment 1, specifically as follows:
the glycerol with the concentration of 95 percent reacts with chlorine-containing tail gas from a paraffin workshop and a prepared catalyst with the flow rate of 2000kg/h in a chlorohydrination reaction kettle, and the temperature of the reaction kettle is controlled at 130 ℃. And (3) introducing the dichloropropanol from the reaction kettle into a rectifying tower for primary distillation, controlling the temperature at the bottom of the rectifying tower to be 155 ℃, and collecting the dichloropropanol, water and hydrochloric acid distilled from the top of the tower to enter the next link. Returning the high-boiling-point substances (including glycerol, dichloropropanol and monochloropropaneol) at the bottom of the tower to the chlorohydrination reaction kettle again for continuous reaction. And the gas phase condensate of the chlorination reaction kettle and the material from the top of the distillation tower enter the same storage tank together for further use.
The dichloropropanol, the water and the hydrochloric acid distilled out for the first time enter a mixer for mixing reaction at the flow rate of 4m/h and 25% of the prepared calcium hydroxide aqueous solution in advance according to the proportion of 1:3, then the mixture is sent into a saponification tower for saponification reaction, the saponification reaction temperature is controlled at 105 ℃, and the primary ECH coming out from the top of the saponification tower is collected. The concentration of the calcium chloride solution from the bottom of the saponification tower is about 15%, and the calcium chloride solution is subjected to pressure filtration and then concentrated into 40% calcium chloride solution by a first-effect device and a second-effect device; finally, concentrating again by climbing a film to ensure that the concentration reaches 70 percent; slicing by a slicer, drying, cooling and packaging to obtain qualified calcium chloride solid.
The primary ECH from the top of the saponification tower contains a large amount of water, so that the ECH is obtained by removing the water through a water removal tower, and the temperature of the water removal tower is controlled at 135 ℃. And performing secondary distillation on the ECH in a rectifying tower to obtain a finished product, wherein the tower bottom temperature of the secondary distillation rectifying tower is controlled at 145 ℃. The amount of tar produced in this example was 0.8%; the resulting finished ECH had a color quality of 2.5.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive. Furthermore, it should be understood that although the present specification describes embodiments, this does not include only one embodiment, and such description is for clarity only, and those skilled in the art should be able to make the specification as a whole, and the embodiments may be appropriately combined to form other embodiments understood by those skilled in the art.
Claims (10)
1. A process for producing epichlorohydrin by using chlorinated paraffin chlorine-containing tail gas through a glycerol method is characterized by comprising the following steps: chlorohydrination of glycerol with gaseous hydrogen chloride in a reaction kettle, at least one distillation, and saponification of the obtained fraction with alkali liquor to obtain epichlorohydrin.
2. The process for producing epichlorohydrin by using chlorinated paraffin chlorine-containing tail gas in a glycerol method according to claim 1, which is characterized in that: the method comprises the following steps:
1) chlorohydrination of glycerol: carrying out chlorohydrination reaction on glycerol, chlorine-containing tail gas from a paraffin production workshop and a prepared catalyst in a chlorohydrination reaction kettle to obtain dichloropropanol;
2) primary distillation: dichlorohydrin obtained by chlorohydrination of glycerol is distilled by a rectifying tower to obtain the dichlorohydrin, water and hydrochloric acid;
3) saponification reaction: reacting dichloropropanol, water and hydrochloric acid obtained by primary distillation with a prepared calcium hydroxide aqueous solution in a mixer according to a certain proportion, and then sending the mixture into a saponification tower for saponification reaction to obtain primary epichlorohydrin;
4) dewatering: sending the primary epoxy chloropropane obtained by saponification into a dewatering tower to remove water, and obtaining a semi-finished product of epoxy chloropropane;
5) secondary distillation: and (4) sending the semi-finished product of the epoxy chloropropane obtained after the water removal into the rectifying tower again for secondary distillation to obtain the finished product of the epoxy chloropropane.
3. The process for producing epichlorohydrin by using chlorinated paraffin chlorine-containing tail gas in a glycerol method according to claim 2, which is characterized in that: in the step 1), the concentration of the glycerol is 95%, and the flow rate of the glycerol is 2000 kg/h; the inlet flow of the chlorine-containing tail gas from the paraffin workshop is 2000 kg/h.
4. The process for producing epichlorohydrin by using chlorinated paraffin chlorine-containing tail gas in a glycerol method according to claim 2, which is characterized in that: in the step 1), the catalyst is a composite chlorination catalyst; the weight ratio of the glycerol to the glycerol is 1: 0.1-0.5.
5. The process for producing epichlorohydrin by using chlorinated paraffin chlorine-containing tail gas in a glycerol method according to claim 2, which is characterized in that: in the step 1), chlorohydrination and chlorination reaction temperature of the glycerol are controlled to be 100-140 ℃.
6. The process for producing epichlorohydrin by using chlorinated paraffin chlorine-containing tail gas in a glycerol method according to claim 2, which is characterized in that: in the step 2), the temperature of the bottom of the primary distillation tower is controlled to be 145-155 ℃.
7. The process for producing epichlorohydrin by using chlorinated paraffin chlorine-containing tail gas in a glycerol method according to claim 2, which is characterized in that: in the step 3), the concentration of the calcium hydroxide aqueous solution used in the saponification reaction is 25%; and (3) carrying out dry distillation on the dichloropropanol, the water and the hydrochloric acid at the flow rate of 4m/h, and mixing the mixture with the calcium hydroxide aqueous solution at the ratio of 1: 1-3, wherein the reaction temperature of the saponification tower is controlled to be 95-105 ℃.
8. The process for producing epichlorohydrin by using chlorinated paraffin chlorine-containing tail gas in a glycerol method according to claim 2, which is characterized in that: in the step 4), the dewatering temperature is controlled to be 125-135 ℃.
9. The process for producing epichlorohydrin by using chlorinated paraffin chlorine-containing tail gas in a glycerol method according to claim 2, which is characterized in that: in the step 5), the temperature of the bottom of the secondary distillation tower is controlled to be 135-145 ℃.
10. The process for producing epichlorohydrin by using chlorinated paraffin chlorine-containing tail gas in a glycerol method according to claim 2, which is characterized in that: also comprises a calcium chloride recovery process; carrying out filter pressing and concentration equipment on the calcium chloride solution generated by the saponification reaction in the step 3) to obtain a calcium chloride solution with the concentration of 40%; concentrating again by climbing film to make its concentration reach 70%; finally, slicing by a slicer, drying and cooling to form calcium chloride solid with qualified quality.
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| WO2022155779A1 (en) * | 2021-01-19 | 2022-07-28 | 汇智工程科技股份有限公司 | Preparation process for epichlorohydrin |
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| CN103333047A (en) * | 2013-07-09 | 2013-10-02 | 南京奥凯化工科技有限公司 | Preparation method of dichloropropanol |
| CN103709124A (en) * | 2013-12-06 | 2014-04-09 | 中国天辰工程有限公司 | Method for producing epoxy chloropropane |
| CN104560197A (en) * | 2014-12-23 | 2015-04-29 | 丹阳市助剂化工厂有限公司 | Tail gas processing process of chlorinated paraffin |
| CN106477525A (en) * | 2016-09-26 | 2017-03-08 | 常州大学 | A kind of chlorination tail gas hydrogen chloride dechlorination gas purifying method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2022155779A1 (en) * | 2021-01-19 | 2022-07-28 | 汇智工程科技股份有限公司 | Preparation process for epichlorohydrin |
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