CN108373400B - Acetylene method chloroethylene synthesis process - Google Patents
Acetylene method chloroethylene synthesis process Download PDFInfo
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Abstract
The invention discloses a vinyl chloride synthesis process by an acetylene method, which comprises the following steps: acetylene is mixed with hydrogen chloride in proportion in a primary mixer through an acetylene flame arrester; preheating mixed gas accounting for 20-90% of the volume ratio of the mixed gas by a primary preheater, and then, entering a front converter for vinyl chloride synthesis; preheating the mixed gas accounting for 80-10% of the volume ratio of the gas by a secondary preheater, and mixing the preheated mixed gas with the mixed gas out of the pre-converter in a secondary mixer; and (4) the gas after secondary mixing enters a rear converter, vinyl chloride synthesis is carried out again, crude vinyl chloride is generated through reaction, and the mixed gas enters a post-treatment system. The catalyst of the front and rear converters of the catalyst does not need to be pumped and turned over, so that the operation rate of equipment is improved, the production cost is reduced, the loss of the catalyst caused by pumping and turning over is reduced, and the environment is protected; the mixed gas is introduced into the post-converter, the pressure of the system is increased, the conversion of the acetylene is promoted, the synthesis of the vinyl chloride is facilitated, the conversion rate is increased, and the service life of the catalyst is prolonged.
Description
Technical Field
The invention relates to the technical field of chloroethylene synthesis, in particular to a chloroethylene synthesis process by an acetylene method.
Background
The prior processes for preparing chloroethylene comprise an acetylene method and an ethylene method, and due to the raw material conditions, most of China adopts the acetylene method to prepare chloroethylene, namely acetylene gas and hydrogen chloride gas are subjected to a synthesis reaction under the action of a mercuric chloride catalyst taking activated carbon as a carrier to generate chloroethylene. The existing vinyl chloride synthesis technology is shown in fig. 1, and is characterized in that acetylene is mixed with hydrogen chloride in a mixer according to a certain proportion through an acetylene flame arrester, the mixture is preheated to 70-80 ℃ through a preheater, and then the mixture sequentially enters a series two-section converter (a front converter and a rear converter respectively) filled with a mercury chloride catalyst taking activated carbon as a carrier to carry out vinyl chloride synthesis, crude vinyl chloride is generated through reaction, and mixed gas enters a post-treatment system. 20-30% of acetylene contained in the gas at the outlet of the front converter is not reacted, and the gas enters the rear converter to continue reacting, so that the content of acetylene at the outlet is controlled to be below 2%. The rear converter is filled with a mercury chloride catalyst with high activity and new active carbon as a carrier, and the front converter is filled with a mercury chloride catalyst with lower activity and active carbon as a carrier (namely, an old mercury chloride catalyst which is replaced by the rear converter through pumping turnover).
The traditional process has the following defects: 1) when the two-section type converter is connected in series to operate, the hydrogen chloride combined with the active center of the mercuric chloride catalyst taking the active carbon as the carrier can not be supplemented in time due to constant material ratio and pressure control, so that the active center is combined with acetylene, and carbonization reaction is carried out at a high temperature for a long time, so that the active center of the catalyst loses activity due to carbon deposition, the service life of the catalyst is shortened, and the yield of a single converter is not improved; 2) the two-section type converter connected in series operates, in order to reduce the operating cost of the catalyst, the mercury chloride catalyst with activated carbon as a carrier needs to be pumped and turned over, and in the pumping and turning over process, the activated carbon carrier has large damage amount due to the problem of self strength and has certain influence on the environment.
Disclosure of Invention
In order to solve the above-mentioned defects existing in the prior art, the present invention aims to provide a vinyl chloride synthesis process by an acetylene method.
The invention is realized by the following technical scheme.
A vinyl chloride synthesis process by an acetylene method comprises the following steps:
1) mixing acetylene and hydrogen chloride which pass through an acetylene flame arrester in a primary mixer according to the molar ratio of the acetylene to the hydrogen chloride of 1 (1.05-1.15);
2) preheating mixed gas accounting for 20-90% of the total mixed gas by a primary preheater, and then entering a front converter filled with a catalyst to synthesize vinyl chloride; preheating mixed gas accounting for 80-10% of the total mixed gas by a secondary preheater, and mixing the preheated mixed gas with the mixed gas out of the pre-converter in a secondary mixer;
3) and the gas after secondary mixing enters a post converter filled with a catalyst, vinyl chloride synthesis is carried out again to generate crude vinyl chloride, and the mixed gas enters a post-treatment system.
Further, in the step 2), the temperature of the mixed gas preheated by the primary preheater is 80-120 ℃.
Further, the temperature of the gas discharged from the primary mixer is-10-45 ℃; the temperature of the gas discharged from the secondary mixer is 90-150 ℃.
Further, the converter controls the reaction temperature to be 90-180 ℃ through circulating water.
Further, the catalyst is one or a mixture of more of mercuric chloride, gold chloride, palladium chloride, copper chloride, silver chloride, bismuth chloride, nickel chloride, lead chloride, tin chloride, platinum chloride, rhodium chloride, molybdenum chloride, tungsten chloride, barium chloride and zinc chloride.
Further, the purity of the acetylene gas is more than or equal to 98.5 percent.
Furthermore, the purity of the hydrogen chloride is more than or equal to 94 percent, and free chlorine is not contained.
The purity of the prepared chloroethylene is not less than 85.3%, the acetylene content is not more than 2.0%, the oxygen content is not more than 2.3%, the chlorine content is not more than 5.7%, and the dichloroethane content is not more than 0.001%.
The invention has the following beneficial effects:
1. the process control is beneficial to improving the capacity of a single converter;
2. the catalyst of the front and rear converters of the catalyst does not need to be pumped and turned over (the catalyst of the background converter is unloaded and is filled into the foreground converter for continuous use), so that the overhaul time is reduced, the equipment operation rate is improved, the production cost is reduced, the loss of the catalyst caused by pumping and turning is reduced, and the environment is protected;
3. after the process, mixed gas is introduced into the converter, the system pressure is increased, the conversion of acetylene is promoted, and the conversion rate is increased.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention:
FIG. 1 is a prior art vinyl chloride synthesis process flow;
FIG. 2 is a process flow of vinyl chloride synthesis according to the present invention.
Detailed Description
The present invention will be described in detail with reference to specific examples, which are provided herein for the purpose of illustration and description, but are not to be construed as limiting the invention.
As shown in fig. 2, the acetylene-method vinyl chloride synthesis process of the invention comprises the following steps:
1) mixing acetylene and hydrogen chloride which pass through an acetylene flame arrester in a primary mixer according to the molar ratio of the acetylene (the purity of acetylene gas is more than or equal to 98.5%) to the hydrogen chloride (the purity of the hydrogen chloride is more than or equal to 94% and free chlorine is not contained) of 1 (1.05-1.15); the temperature of the gas discharged from the primary mixer is-10-45 ℃;
2) preheating mixed gas accounting for 20-90% of the total mixed gas by a primary preheater (the temperature of the mixed gas preheated by the primary preheater is 80-120 ℃), and then entering a front converter filled with a catalyst (mercury chloride, gold chloride, palladium chloride, copper chloride, silver chloride, bismuth chloride, nickel chloride, lead chloride, tin chloride, platinum chloride, rhodium chloride, molybdenum chloride, tungsten chloride, barium chloride and zinc chloride) to carry out chloroethylene synthesis; preheating mixed gas accounting for 80-10% of the total mixed gas by a secondary preheater, and mixing the preheated mixed gas with the mixed gas discharged from the pre-converter in a secondary mixer (the temperature of the gas discharged from the secondary mixer is 90-150 ℃);
3) and (3) introducing the gas after secondary mixing into a post-converter filled with a catalyst (mercury chloride, gold chloride, palladium chloride, copper chloride, silver chloride, bismuth chloride, nickel chloride, lead chloride, tin chloride, platinum chloride, rhodium chloride, molybdenum chloride, tungsten chloride, barium chloride and zinc chloride), controlling the reaction temperature of the converter at 90-180 ℃ through circulating water to synthesize chloroethylene, reacting to generate crude chloroethylene, and introducing the mixed gas into a post-treatment system.
The method comprises the steps that acetylene and hydrogen chloride are mixed through an acetylene flame arrester and a primary mixer (the molar ratio of acetylene to hydrogen chloride is 1: 1.05-1.15) and are divided into two paths, wherein one path of mixed gas (accounting for 20-90% of the total amount) enters a primary preheater for preheating and then enters a front converter filled with a catalyst, the mixed gas subjected to vinyl chloride synthesis and the other path of mixed gas (accounting for 80-10% of the total amount) preheated through a secondary preheater enter a secondary mixer for mixing and then enter a rear converter for vinyl chloride synthesis, the reaction temperature of the converter is controlled to be 90-180 ℃ through circulating water, and gas phase reaction is carried out under the catalytic action of the catalyst to generate vinyl chloride; and finally, the mixed gas enters an after-treatment system.
Mixing the acetylene flame arrester and hydrogen chloride through a primary mixer, controlling the total mole ratio of the hydrogen chloride to the acetylene, preheating part of mixed gas for the first time, and then feeding the preheated gas into a front converter filled with a catalyst to synthesize vinyl chloride; then, after a part of the mixed gas preheated by the secondary preheater is further mixed with the mixed gas containing chloroethylene in the converter before the mixed gas is discharged, the mixed gas enters a post-converter filled with a catalyst to fully react, and then chloroethylene synthesis is carried out again. According to the invention, mixed gas is introduced into the rear converter, the system pressure is increased, the conversion of acetylene is promoted, the conversion rate is increased, and the conversion rate of the whole converter can reach 99.7%; the process can adjust the gas content of the converter before and after entering, efficiently use the catalyst, and prolong the service life of the catalyst to over 9000 hours.
Specific examples are given below to further illustrate the present invention.
Example 1
Mixing acetylene and hydrogen chloride which pass through an acetylene flame arrester in a primary mixer according to the molar ratio of the acetylene to the hydrogen chloride of 1:1.05 to ensure that the gas temperature is-10 ℃; preheating the mixed gas accounting for 20 percent of the volume ratio of the mixed gas by a primary preheater to reach the temperature of 80 ℃, and introducing the mixed gas into a front converter filled with a gold chloride catalyst; preheating mixed gas accounting for 80% of the total mixed gas by a secondary preheater, and mixing the preheated mixed gas with the mixed gas discharged from the pre-converter in a secondary mixer to ensure that the temperature of the mixed gas is 90 ℃; and the gas after secondary mixing enters a post converter filled with a gold chloride catalyst, the converter performs chloroethylene synthesis by controlling the reaction temperature to be 90 ℃ through circulating water, crude chloroethylene is generated through reaction, and the mixed gas enters a post-treatment system. The conversion of the converter of this example was 99.2%.
Example 2
Mixing acetylene and hydrogen chloride which pass through an acetylene flame arrester in a primary mixer according to the molar ratio of the acetylene to the hydrogen chloride of 1:1.1 to ensure that the gas temperature is 45 ℃; preheating mixed gas accounting for 60% of the volume ratio of the mixed gas by a primary preheater to ensure that the temperature of the mixed gas is 100 ℃, and introducing the mixed gas into a front converter filled with a mercuric chloride catalyst; preheating mixed gas accounting for 40% of the total mixed gas by a secondary preheater, and mixing the preheated mixed gas with the mixed gas discharged from the pre-converter in a secondary mixer to ensure that the temperature is 120 ℃; and the gas after secondary mixing enters a post converter filled with a mercuric chloride catalyst, the converter performs chloroethylene synthesis reaction at 140 ℃ by controlling the reaction temperature through circulating water to generate crude chloroethylene, and the mixed gas enters a post-treatment system. The conversion of the converter of this example was 99.7%.
Example 3
Mixing acetylene and hydrogen chloride which pass through an acetylene flame arrester in a primary mixer according to the molar ratio of the acetylene to the hydrogen chloride of 1:1.15 to ensure that the gas temperature is 25 ℃; preheating mixed gas accounting for 90% of the volume ratio of the mixed gas by a primary preheater to ensure that the temperature of the mixed gas is 120 ℃, and introducing the mixed gas into a front converter filled with copper chloride and silver chloride catalysts; preheating mixed gas accounting for 10 percent of the total mixed gas by a secondary preheater, and mixing the preheated mixed gas with the mixed gas discharged from the pre-converter in a secondary mixer to ensure that the temperature reaches 150 ℃; and the gas after secondary mixing enters a post converter filled with copper chloride and silver chloride catalysts, the converter performs chloroethylene synthesis by controlling the reaction temperature to be 180 ℃ through circulating water, crude chloroethylene is generated through reaction, and the mixed gas enters a post-treatment system. The conversion of the converter of this example was 99.4%.
Example 4
Mixing acetylene and hydrogen chloride which pass through an acetylene flame arrester in a primary mixer according to the molar ratio of the acetylene to the hydrogen chloride of 1:1.08 to ensure that the gas temperature is 5 ℃; preheating mixed gas accounting for 40% of the volume ratio of the mixed gas by a primary preheater to enable the temperature of the mixed gas to be 90 ℃, and introducing the mixed gas into a front converter filled with palladium chloride, nickel chloride and bismuth chloride catalysts; preheating mixed gas accounting for 60 percent of the total mixed gas by a secondary preheater, and mixing the preheated mixed gas with the mixed gas discharged from the pre-converter in a secondary mixer to ensure that the temperature reaches 105 ℃; and the gas after secondary mixing enters a post-converter filled with palladium chloride, nickel chloride and bismuth chloride catalysts, the converter performs chloroethylene synthesis by controlling the reaction temperature to be 115 ℃ through circulating water, crude chloroethylene is generated through reaction, and the mixed gas enters a post-treatment system. The conversion of the converter of this example was 99.5%.
Example 5
Mixing acetylene and hydrogen chloride which pass through an acetylene flame arrester in a primary mixer according to the molar ratio of the acetylene to the hydrogen chloride of 1:1.13 to ensure that the gas temperature is 35 ℃; preheating mixed gas accounting for 75% of the volume ratio of the mixed gas by a primary preheater to ensure that the temperature of the mixed gas is 110 ℃, and introducing the mixed gas into a front converter filled with a mixed catalyst of tin chloride, lead chloride and platinum chloride; preheating mixed gas accounting for 25 percent of the total mixed gas by a secondary preheater, and mixing the preheated mixed gas with the mixed gas discharged from the pre-converter in a secondary mixer to ensure that the temperature reaches 135 ℃; and (3) feeding the gas after secondary mixing into a post-converter filled with a mixed catalyst of tin chloride, lead chloride and platinum chloride, controlling the reaction temperature of the post-converter to be 165 ℃ through circulating water to synthesize chloroethylene, reacting to generate crude chloroethylene, and feeding the mixed gas into a post-treatment system. The conversion of the converter of this example was 99.4%.
The invention only provides an example of vinyl chloride conversion by using different catalysts, and the rhodium chloride, molybdenum chloride, tungsten chloride, barium chloride and zinc chloride catalysts listed in the technical scheme of the invention can achieve the same conversion effect in vinyl chloride synthesis as the catalysts listed in the example.
The results of the relevant performance tests of the crude vinyl chloride are given in table 1 below.
TABLE 1 comparison of the results of the relevant Performance tests on crude vinyl chloride
As can be seen from the above examples, the vinyl chloride produced by the process of the present invention has a purity of not less than 85.3%, an acetylene content of not more than 2.0%, an oxygen content of not more than 2.3%, a chlorine content of not more than 5.7%, and a dichloroethane content of not more than 0.001%.
The present invention is not limited to the above-mentioned embodiments, and based on the technical solutions disclosed in the present invention, those skilled in the art can make some substitutions and modifications to some technical features without creative efforts according to the disclosed technical contents, and these substitutions and modifications are all within the protection scope of the present invention.
Claims (8)
1. The acetylene-method vinyl chloride synthesis process is characterized by comprising the following steps:
1) mixing acetylene and hydrogen chloride which pass through an acetylene flame arrester in a primary mixer according to the molar ratio of the acetylene to the hydrogen chloride of 1 (1.05-1.15);
2) preheating mixed gas accounting for 20-90% of the total mixed gas by a primary preheater, and then entering a front converter filled with a catalyst to synthesize vinyl chloride; preheating mixed gas accounting for 80-10% of the total mixed gas by a secondary preheater, and mixing the preheated mixed gas with the mixed gas out of the pre-converter in a secondary mixer;
3) and the gas after secondary mixing enters a post converter filled with a catalyst, vinyl chloride synthesis is carried out again to generate crude vinyl chloride, and the mixed gas enters a post-treatment system.
2. The acetylene-method vinyl chloride synthesis process according to claim 1, wherein in the step 2), the temperature of the mixed gas preheated by the primary preheater is 80-120 ℃.
3. The acetylene-process vinyl chloride synthesis process according to claim 1, wherein the temperature of the gas discharged from the primary mixer is-10 to 45 ℃; the temperature of the gas discharged from the secondary mixer is 90-150 ℃.
4. The acetylene-process vinyl chloride synthesis process according to claim 1, wherein the reaction temperature of the converter is controlled to be 90-180 ℃ by circulating water.
5. The acetylene-process vinyl chloride synthesis process according to claim 1, wherein the catalyst is one or a mixture of mercury chloride, gold chloride, palladium chloride, copper chloride, silver chloride, bismuth chloride, nickel chloride, lead chloride, tin chloride, platinum chloride, rhodium chloride, molybdenum chloride, tungsten chloride, barium chloride or zinc chloride.
6. The acetylene-process vinyl chloride synthesis process according to claim 1, wherein the purity of the acetylene gas is not less than 98.5%.
7. The acetylene-process vinyl chloride synthesis process according to claim 1, wherein the purity of the hydrogen chloride is not less than 94% and free chlorine is not contained.
8. The process of claim 1, wherein the vinyl chloride product has a purity of not less than 85.3%, an acetylene content of not more than 2.0%, an oxygen content of not more than 2.3%, a chlorine content of not more than 5.7%, and a dichloroethane content of not more than 0.001%.
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| CN108373400B (en) * | 2018-02-05 | 2020-06-30 | 陕西北元化工集团股份有限公司 | Acetylene method chloroethylene synthesis process |
| CN110963883B (en) * | 2018-09-28 | 2023-02-28 | 中国石油化工股份有限公司 | Method for hydrochlorinating acetylene |
| CN112159303B (en) * | 2020-08-27 | 2023-10-24 | 鄂尔多斯市瀚博科技有限公司 | Vinyl chloride synthesis process suitable for mercury-free catalyst |
| CN115572207B (en) * | 2022-10-19 | 2024-08-02 | 鄂尔多斯市瀚博科技有限公司 | Method for preparing chloroethylene by reducing acetylene hydrochlorination byproducts through gold-based catalysis |
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