CN102816045B - Method for synthesizing chloromethane by tail gas generated during chloroacetic acid production - Google Patents

Method for synthesizing chloromethane by tail gas generated during chloroacetic acid production Download PDF

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CN102816045B
CN102816045B CN201210326303.3A CN201210326303A CN102816045B CN 102816045 B CN102816045 B CN 102816045B CN 201210326303 A CN201210326303 A CN 201210326303A CN 102816045 B CN102816045 B CN 102816045B
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CN102816045A (en
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刘玉敏
刘宝树
胡永其
魏士东
张文娇
花秀艳
李娇
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Hebei University of Science and Technology
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Abstract

The invention relates to a method for synthesizing chloromethane by tail gas generated during chloroacetic acid production. Firstly, the tail gas which is generated during chloroacetic acid production and contains hydrogen chloride is enabled to sequentially pass through a hydrochloric acid gas washing device, an acetic acid gas washing device and an adsorption device which contains solid adsorbents to be subjected to a purification treatment, then the tail gas is premixed with methanol to obtain a mixture, and the mixture is fed to a synthesis reactor to generate the chloromethane under the action of catalysts. The gas after the reaction is respectively subjected to washing, alkaline washing and concentrated sulfuric acid drying to obtain a high purity chloromethane product. The method for synthesizing the chloromethane by the tail gas generated during chloroacetic acid production has the advantages that the equipment investment is small, the operation is simple, the efficiency is high, raw materials are easy to obtain, and the like.

Description

A kind of method of the tail gas synthesis methyl chloride utilized in production of chloroacetic acid
Technical field
The invention belongs to chemical technology field, relate to a kind of method of the tail gas synthesis methyl chloride utilized in production of chloroacetic acid.
Background technology
Methyl chloride is a kind of important organic synthesis intermediate, and methyl chloride product enters the ripening stage in developed country, is domesticly in important development stage.The current main application of monochloro methane produces methyl chlorosilane, methyl atmosphere silane is the monomer of synthesizing organo-silicon material, be widely used in the industries such as building, weaving, electronics, electrical equipment, machinery, traffic, chemical industry, medical treatment, food, Aeronautics and Astronautics, due to current industry and social development, in for some time from now on, as the methane chloride production of methyl atmosphere silane main raw material and trade still in zooming trend.The industrial production of methyl chloride is mainly with the production technique that methyl alcohol and hydrogenchloride are raw material, the hydrogenchloride that the hydrogen chloride gas adopted needs synthesis method to produce or be raw material by the hydrogenchloride that concentrated hydrochloric acid high temperature deep analysis obtains is generally higher to the purity requirement of hydrogen chloride gas.The hydrogenchloride of organic chloride building-up process by-product, due to containing more organic impurity, have not been reported the synthesis for methyl chloride.
Most production of chloroacetic acid enterprise of China all adopts acetic acid chlorination process, and the composition producing tail gas is mainly hydrogenchloride.Be all absorb generation by-product hydrochloric acid by water to carry out sale at low prices at present, because the amount of by-product is very large, and wherein containing organic impurity, limit it and use, usually occur unsalable phenomenon, have impact on the further expansion of production of chloroacetic acid scale.If it directly to be carried out scene digestion, produce high value-added product further, Mono Chloro Acetic Acid industrial expansion will be conducive to, be also conducive to eliminating the environmental pollution hidden danger caused by the existence of excessive hydrochloric acid simultaneously.
The production processes of chloroacetic acid of China all adopts SULPHUR POWDER to be catalyzer, the hydrogen chloride tail gas of by-product is generally containing the impurity such as catalyzer SULPHUR POWDER and Acetyl Chloride 98Min., chloroacetyl chloride and sulfocompound, the band membership of these materials affects the quality of methyl chloride building-up reactions and product, therefore must purify before the reaction this tail gas.
Summary of the invention
The present invention solves existing problem in the art, provides a kind of method of the tail gas synthesis methyl chloride utilized in production of chloroacetic acid, to remove the impurity in production of chloroacetic acid tail gas, uses it for the synthesis of methyl chloride.
The present invention is achieved by the following technical solutions:
The method of a kind of tail gas synthesis methyl chloride utilized in production of chloroacetic acid of the present invention, it comprises the following steps:
A. from the tail gas of containing hydrogen chloride in production processes of chloroacetic acid, first enter compressor gas is compressed, then enter the bottom of acetic acid washing tower, the tail gas of containing hydrogen chloride and acetum counter current contact in acetic acid washing tower, to absorb in gas the material being dissolved in acetic acid.
B. acetic acid washing tower top gas out in described step a, enters the bottom of hydrochloric acid washing tower, and gas and hydrochloric acid soln counter current contact in hydrochloric acid washing tower, to absorb material water-soluble in gas.
C. hydrochloric acid washing tower top gas out in described step b, enters gas adsorbing device, to adsorb the sulfur-containing impurities in the tail gas of containing hydrogen chloride, carries out deep purifying to gas.
D. the methanol gas in described step c after cleaned gas and heating, in a mixer after pre-mixing, enters in the reactor containing liquid-phase catalyst and chemical reactive synthesis methyl chloride occurs.
E. described steps d carries out condensing reflux by the reactor methyl chloride gas that contains out through reflux condensate device, enter water wash column subsequently, enter soda-wash tower again, enter first step sulfuric acid tower, second stage sulfuric acid tower, third stage sulfuric acid tower afterwards successively, after depickling, dehydration and purifying treatment are carried out to methyl chloride gas, obtain highly purified methyl chloride gas.
F. the methyl chloride gas that obtains of described step e is after compressor, then enters water cooler and carry out cooling and condensation obtains methyl chloride liquid product, enters the storage of liquid chlorine methane storage tank.
Preferably, the method for described a kind of tail gas synthesis methyl chloride utilized in production of chloroacetic acid, the pressure of tail gas containing hydrogen chloride after compressor described in step a brings up to 0.3-0.8MPa.Acetic acid scrubber tower described in step a is two sections of packing towers, and service temperature is 15 DEG C ~ 40 DEG C.
Preferably, the method for described a kind of tail gas synthesis methyl chloride utilized in production of chloroacetic acid, the hydrochloric acid washing tower described in step b is two sections of packing towers, and service temperature is 15 DEG C ~ 40 DEG C.
Preferably, the method for described a kind of tail gas synthesis methyl chloride utilized in production of chloroacetic acid, the solid adsorbent in the gas adsorbing device described in step c is one or more in aluminum oxide, molecular sieve, gac, silica gel.
Preferably, the method for described a kind of tail gas synthesis methyl chloride utilized in production of chloroacetic acid, the reactor described in steps d is glass lined reaction vessel, and temperature of reaction is 130 ~ 160 DEG C, and working pressure is 0.1 ~ 0.5MPa.Liquid-phase catalyst described in steps d is 50% ~ 85% zinc chloride and/or 5% ~ 10% nickel chloride aqueous solution.
Preferably, the method for described a kind of tail gas synthesis methyl chloride utilized in production of chloroacetic acid, the Alkali absorption liquid used of the soda-wash tower described in step e is the aqueous sodium hydroxide solution of 10% ~ 60%.Third stage sulfuric acid tower described in step e sour absorption liquid used is the vitriol oil of 93% or more.
Preferred further, the method for described a kind of tail gas synthesis methyl chloride utilized in production of chloroacetic acid, it is characterized in that, it specifically comprises the following steps:
A. from the tail gas of containing hydrogen chloride in production processes of chloroacetic acid, first enter compressor gas is carried out being compressed to 0.5MPa, then enter the bottom of acetic acid washing tower, the tail gas of containing hydrogen chloride and acetum counter current contact in acetic acid washing tower, to absorb in gas the material being dissolved in acetic acid.The service temperature of acetic acid washing tower is 30 DEG C.The tail gas of containing hydrogen chloride is discharged from washing tower top after acetic acid washing, and acetic acid is squeezed into circulation device by pump again after discharging from bottom and recycled.
B. from a step acetic acid scrubber tower top gas out, enter the bottom of hydrochloric acid washing tower, gas and hydrochloric acid soln counter current contact in hydrochloric acid washing tower, to absorb material water-soluble in gas.The service temperature of hydrochloric acid washing tower is 30 DEG C.The tail gas of containing hydrogen chloride is discharged from washing tower top after salt acid elution, and hydrochloric acid is squeezed into circulation device by pump again after discharging from bottom and recycled.
C. from b step hydrochloric acid washing tower top gas out, enter gas adsorbing device, to adsorb the sulfur-containing impurities in the tail gas of containing hydrogen chloride, deep purifying is carried out to gas.Gas adsorbing device inside is filled with molecular sieve and aluminum oxide.
D. the methanol gas in step c after cleaned gas and heating is in a mixer after pre-mixing, enters in the reactor of the aqueous solution liquid-phase catalyst containing 60% zinc chloride and 10% nickelous chloride and chemical reactive synthesis methyl chloride occurs.The service temperature of reactor is 150 DEG C, and working pressure is 0.3MPa.
E. described steps d carries out condensing reflux by the reactor methyl chloride gas that contains out through reflux condensate device, enter water wash column subsequently, then soda-wash tower is entered, enter first step sulfuric acid tower, second stage sulfuric acid tower, third stage sulfuric acid tower more successively, after depickling, dehydration and purifying treatment are carried out to methyl chloride gas, obtain highly purified methyl chloride gas.Soda-wash tower Alkali absorption liquid used is the aqueous sodium hydroxide solution of 50%.Sulfuric acid tower sour absorption liquid used is the vitriol oil of 95%, enters second stage sulfuric acid tower from third stage sulfuric acid tower sulfuric acid absorption liquid out, enters second stage sulfuric acid tower from second stage sulfuric acid tower sulfuric acid absorption liquid out.
F. the methyl chloride gas that described step e obtains is compressed to after 0.7MPa through compressor, enters water cooler and carries out cooling and condensation obtains methyl chloride liquid product, finally enters the storage of liquid chlorine methane storage tank.
The present invention compared with prior art has following significant advantage:
1. equipment operates at ambient pressure, invests little, and equipment is simple, and technical process is short.
2. easily quiet run and control, simple to operate, expense is low.
3. product separation is simple, thorough, and the product after being separated can recycle.
4. production process environmental pollution is little.
5. treated hydrogen chloride tail gas purity is high, quality good, and the hydrogenchloride after process can be used for methanolic hydrogen chloride synthesis methyl chloride technique.
In a word, the present invention has that technique is simple, facility investment is little, simple to operate, the manageable feature of good stability, appearance.The hydrogen chloride tail gas utilizing this technique that poor quality in Mono Chloro Acetic Acid technique, purity can be made low obtains high value and utilizes in the methyl chloride synthesis of synthesis high added value.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of the inventive method.
Each part description in figure:
1, production processes of chloroacetic acid tail gas containing hydrogen chloride; 2, compressor; 3 acetic acid washing towers; 4, hydrochloric acid washing tower; 5, gas adsorbing device; Methyl alcohol after 6 heating and gasifyings; 7, mixing tank; 8, reactor; 9, reflux condensate device; 10, water wash column; 11, soda-wash tower; 12, first step sulfuric acid tower; 13, second stage sulfuric acid tower; 14, third stage sulfuric acid tower; 15, compressor; 16, cooler condenser; 17, methyl chloride storage tank.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail.
Embodiment 1
A. from the tail gas 1 of containing hydrogen chloride in production processes of chloroacetic acid, first enter compressor 2 gas is carried out being compressed to 0.3MPa, then the bottom of acetic acid washing tower 3 is entered, the tail gas 1 of containing hydrogen chloride and acetum counter current contact in acetic acid washing tower 3, to absorb in gas the material being dissolved in acetic acid.The service temperature of acetic acid washing tower 3 is 15 DEG C.The tail gas 1 of containing hydrogen chloride is discharged from washing tower top after acetic acid washing, and acetic acid is squeezed into circulation device by pump again after discharging from bottom and recycled.
B. from a step acetic acid scrubber tower 3 top gas out, enter the bottom of hydrochloric acid washing tower 4, gas and hydrochloric acid soln counter current contact in hydrochloric acid washing tower 4, to absorb material water-soluble in gas.The service temperature of hydrochloric acid washing tower 4 is 15 DEG C.The tail gas 1 of containing hydrogen chloride is discharged from washing tower top after salt acid elution, and hydrochloric acid is squeezed into circulation device by pump again after discharging from bottom and recycled.
C. from b step hydrochloric acid washing tower 4 top gas out, enter gas adsorbing device 5, to adsorb the sulfur-containing impurities in the tail gas 1 of containing hydrogen chloride, deep purifying is carried out to gas.Gas adsorbing device 5 inside is filled with gac and silica gel.
D. the methanol gas 6 in step c after cleaned gas and heating in mixing tank 7 after pre-mixing, enters in the reactor 8 containing 50% zinc chloride and 10% nickel chloride aqueous solution liquid-phase catalyst and chemical reactive synthesis methyl chloride occurs.The service temperature of reactor 8 is 130 DEG C, and working pressure is 0.1MPa.
E. described steps d carries out condensing reflux by reactor 8 methyl chloride gas that contains out through reflux condensate device 9, enter water wash column 10 subsequently, then soda-wash tower 11 is entered, enter first step sulfuric acid tower 12, second stage sulfuric acid tower 13, third stage sulfuric acid tower 14 more successively, after depickling, dehydration and purifying treatment are carried out to methyl chloride gas, obtain highly purified methyl chloride gas.Soda-wash tower 11 Alkali absorption liquid used is the aqueous sodium hydroxide solution of 10%.Sulfuric acid tower 14 sour absorption liquid used is the vitriol oil of 93%, enters second stage sulfuric acid tower 13 from third stage sulfuric acid tower 14 sulfuric acid absorption liquid out, enters second stage sulfuric acid tower 12 from second stage sulfuric acid tower 13 sulfuric acid absorption liquid out.
F. the methyl chloride gas that obtains of described step e is after compressor 15 is compressed to 0.7MPa, enters water cooler 16 and carries out cooling and condensation obtains methyl chloride liquid product, finally enter liquid chlorine methane storage tank 17 and store.
Embodiment 2
A. from the tail gas 1 of containing hydrogen chloride in production processes of chloroacetic acid, first enter compressor 2 gas is carried out being compressed to 0.5MPa, then the bottom of acetic acid washing tower 3 is entered, the tail gas 1 of containing hydrogen chloride and acetum counter current contact in acetic acid washing tower 3, to absorb in gas the material being dissolved in acetic acid.The service temperature of acetic acid washing tower 3 is 30 DEG C.The tail gas 1 of containing hydrogen chloride is discharged from washing tower top after acetic acid washing, and acetic acid is squeezed into circulation device by pump again after discharging from bottom and recycled.
B. from a step acetic acid scrubber tower 3 top gas out, enter the bottom of hydrochloric acid washing tower 4, gas and hydrochloric acid soln counter current contact in hydrochloric acid washing tower 4, to absorb material water-soluble in gas.The service temperature of hydrochloric acid washing tower 4 is 30 DEG C.The tail gas 1 of containing hydrogen chloride is discharged from washing tower top after salt acid elution, and hydrochloric acid is squeezed into circulation device by pump again after discharging from bottom and recycled.
C. from b step hydrochloric acid washing tower 4 top gas out, enter gas adsorbing device 5, to adsorb the sulfur-containing impurities in the tail gas 1 of containing hydrogen chloride, deep purifying is carried out to gas.Gas adsorbing device 5 inside is filled with molecular sieve and aluminum oxide.
D. the methanol gas 6 in step c after cleaned gas and heating in mixing tank 7 after pre-mixing, enters in the reactor 8 of the aqueous solution liquid-phase catalyst containing 60% zinc chloride and 10% nickelous chloride and chemical reactive synthesis methyl chloride occurs.The service temperature of reactor 8 is 150 DEG C, and working pressure is 0.3MPa.
E. described steps d carries out condensing reflux by reactor 8 methyl chloride gas that contains out through reflux condensate device 9, enter water wash column 10 subsequently, then soda-wash tower 11 is entered, enter first step sulfuric acid tower 12, second stage sulfuric acid tower 13, third stage sulfuric acid tower 14 more successively, after depickling, dehydration and purifying treatment are carried out to methyl chloride gas, obtain highly purified methyl chloride gas.Soda-wash tower 11 Alkali absorption liquid used is the aqueous sodium hydroxide solution of 50%.Sulfuric acid tower 14 sour absorption liquid used is the vitriol oil of 95%, enters second stage sulfuric acid tower 13 from third stage sulfuric acid tower 14 sulfuric acid absorption liquid out, enters second stage sulfuric acid tower 12 from second stage sulfuric acid tower 13 sulfuric acid absorption liquid out.
F. the methyl chloride gas that obtains of described step e is after compressor 15 is compressed to 0.7MPa, enters water cooler 16 and carries out cooling and condensation obtains methyl chloride liquid product, finally enter liquid chlorine methane storage tank 17 and store.
Embodiment 3
A. from the tail gas 1 of containing hydrogen chloride in production processes of chloroacetic acid, first enter compressor 2 gas is carried out being compressed to 0.8MPa, then the bottom of acetic acid washing tower 3 is entered, the tail gas 1 of containing hydrogen chloride and acetum counter current contact in acetic acid washing tower 3, to absorb in gas the material being dissolved in acetic acid.The service temperature of acetic acid washing tower 3 is 40 DEG C.The tail gas 1 of containing hydrogen chloride is discharged from washing tower top after acetic acid washing, and acetic acid is squeezed into circulation device by pump again after discharging from bottom and recycled.
B. from a step acetic acid scrubber tower 3 top gas out, enter the bottom of hydrochloric acid washing tower 4, gas and hydrochloric acid soln counter current contact in hydrochloric acid washing tower 4, to absorb material water-soluble in gas.The service temperature of hydrochloric acid washing tower 4 is 40 DEG C.The tail gas 1 of containing hydrogen chloride is discharged from washing tower top after salt acid elution, and hydrochloric acid is squeezed into circulation device by pump again after discharging from bottom and recycled.
C. from b step hydrochloric acid washing tower 4 top gas out, enter gas adsorbing device 5, to adsorb the sulfur-containing impurities in the tail gas 1 of containing hydrogen chloride, deep purifying is carried out to gas.Gas adsorbing device 5 inside is filled with gac.
D. in step c, cleaned gas and the methanol gas 6 after heating after pre-mixing, enter in the reactor 8 containing 85% solder(ing)acid liquid-phase catalyst and chemical reactive synthesis methyl chloride occur in mixing tank 7.The service temperature of reactor 8 is 140 DEG C, and working pressure is 0.5MPa.
E. described steps d carries out condensing reflux by reactor 8 methyl chloride gas that contains out through reflux condensate device 9, enter water wash column 10 subsequently, then soda-wash tower 11 is entered, enter first step sulfuric acid tower 12, second stage sulfuric acid tower 13, third stage sulfuric acid tower 14 more successively, after depickling, dehydration and purifying treatment are carried out to methyl chloride gas, obtain highly purified methyl chloride gas.Soda-wash tower 11 Alkali absorption liquid used is the aqueous sodium hydroxide solution of 60%.Sulfuric acid tower 14 sour absorption liquid used is the vitriol oil of 98%, enters second stage sulfuric acid tower 13 from third stage sulfuric acid tower 14 sulfuric acid absorption liquid out, enters second stage sulfuric acid tower 12 from second stage sulfuric acid tower 13 sulfuric acid absorption liquid out.
F. the methyl chloride gas that obtains of described step e is after compressor 15 is compressed to 0.7MPa, enters water cooler 16 and carries out cooling and condensation obtains methyl chloride liquid product, finally enter liquid chlorine methane storage tank 17 and store.

Claims (6)

1. utilize a method for the tail gas synthesis methyl chloride in production of chloroacetic acid, it is characterized in that, it comprises the following steps:
A. from the tail gas (1) of containing hydrogen chloride in production processes of chloroacetic acid, first enter compressor (2) gas is compressed, then the bottom of acetic acid washing tower (3) is entered, in tail gas (1) and the acetum counter current contact of the middle containing hydrogen chloride of acetic acid washing tower (3), to absorb in gas the material being dissolved in acetic acid;
B. acetic acid washing tower (3) top gas out in described step a, enter the bottom of hydrochloric acid washing tower (4), gas and hydrochloric acid soln counter current contact in hydrochloric acid washing tower (4), to absorb material water-soluble in gas;
C. hydrochloric acid washing tower (4) top gas out in described step b, enters gas adsorbing device (5), to adsorb the sulfur-containing impurities in the tail gas (1) of containing hydrogen chloride, carries out deep purifying to gas;
D. in described step c, cleaned gas and the methanol gas (6) after heating after pre-mixing, enter in the reactor (8) containing liquid-phase catalyst and chemical reactive synthesis methyl chloride occur in mixing tank (7);
E. described steps d carries out condensing reflux by reactor (8) methyl chloride gas that contains out through reflux condensate device (9), enter water wash column (10) subsequently, enter soda-wash tower (11) again, enter first step sulfuric acid tower (12), second stage sulfuric acid tower (13), third stage sulfuric acid tower (14) afterwards successively, after depickling, dehydration and purifying treatment are carried out to methyl chloride gas, obtain methyl chloride gas;
F. the methyl chloride gas that obtains of described step e is after compressor (15), then enters water cooler (16) and carry out cooling and condensation obtains methyl chloride liquid product, enters liquid chlorine methane storage tank (17) storage;
Described liquid-phase catalyst is the aqueous solution containing 60% zinc chloride and 10% nickelous chloride;
The pressure of the tail gas containing hydrogen chloride after compressor (1) described in step a brings up to 0.3-0.8MPa;
Acetic acid scrubber tower (3) described in step a is two sections of packing towers, and service temperature is 15 DEG C ~ 40 DEG C;
Hydrochloric acid washing tower (4) described in step b is two sections of packing towers, and service temperature is 15 DEG C ~ 40 DEG C.
2. the method for a kind of tail gas synthesis methyl chloride utilized in production of chloroacetic acid as claimed in claim 1, the solid adsorbent that it is characterized in that in the gas adsorbing device (5) described in step c is one or more in aluminum oxide, molecular sieve, gac, silica gel.
3. as claimed in claim 1 a kind of utilize in production of chloroacetic acid tail gas synthesis methyl chloride method, it is characterized in that the reactor (8) described in steps d is glass lined reaction vessel, temperature of reaction is 130 ~ 160 DEG C, and working pressure is 0.1 ~ 0.5MPa.
4. the method for a kind of tail gas synthesis methyl chloride utilized in production of chloroacetic acid as claimed in claim 1, is characterized in that soda-wash tower (11) described in step e Alkali absorption liquid used is the aqueous sodium hydroxide solution of 10% ~ 60%.
5. the method for a kind of tail gas synthesis methyl chloride utilized in production of chloroacetic acid as claimed in claim 1, is characterized in that third stage sulfuric acid tower (14) described in step e sour absorption liquid used is the vitriol oil of 93% or more.
6. as claimed in claim 1 a kind of utilize in production of chloroacetic acid tail gas synthesis methyl chloride method, it is characterized in that, it specifically comprises the following steps:
A. from the tail gas (1) of containing hydrogen chloride in production processes of chloroacetic acid, first enter compressor (2) gas is carried out being compressed to 0.5MPa, then the bottom of acetic acid washing tower (3) is entered, in tail gas (1) and the acetum counter current contact of the middle containing hydrogen chloride of acetic acid washing tower (3), to absorb in gas the material being dissolved in acetic acid; The service temperature of acetic acid washing tower (3) is 30 DEG C; The tail gas (1) of containing hydrogen chloride is discharged from washing tower top after acetic acid washing, and acetic acid is squeezed into circulation device by pump again after discharging from bottom and recycled;
B. from a step acetic acid scrubber tower (3) top gas out, enter the bottom of hydrochloric acid washing tower (4), gas and hydrochloric acid soln counter current contact in hydrochloric acid washing tower (4), to absorb material water-soluble in gas; The service temperature of hydrochloric acid washing tower (4) is 30 DEG C; The tail gas (1) of containing hydrogen chloride is discharged from washing tower top after salt acid elution, and hydrochloric acid is squeezed into circulation device by pump again after discharging from bottom and recycled;
C. from b step hydrochloric acid washing tower (4) top gas out, enter gas adsorbing device (5), to adsorb the sulfur-containing impurities in the tail gas (1) of containing hydrogen chloride, deep purifying is carried out to gas; Gas adsorbing device (5) inside is filled with molecular sieve and aluminum oxide;
D. the methanol gas (6) in step c after cleaned gas and heating in the mixing tank (7) after pre-mixing, enters in the reactor (8) of the aqueous solution liquid-phase catalyst containing 60% zinc chloride and 10% nickelous chloride and chemical reactive synthesis methyl chloride occurs; The service temperature of reactor (8) is 150 DEG C, and working pressure is 0.3MPa;
E. described steps d carries out condensing reflux by reactor (8) methyl chloride gas that contains out through reflux condensate device (9), enter water wash column (10) subsequently, then soda-wash tower (11) is entered, enter first step sulfuric acid tower (12), second stage sulfuric acid tower (13), third stage sulfuric acid tower (14) more successively, after depickling, dehydration and purifying treatment are carried out to methyl chloride gas, obtain methyl chloride gas; Soda-wash tower (11) Alkali absorption liquid used is the aqueous sodium hydroxide solution of 50%; Sulfuric acid tower (14) sour absorption liquid used is the vitriol oil of 95%, enter second stage sulfuric acid tower (13) from third stage sulfuric acid tower (14) sulfuric acid absorption liquid out, enter second stage sulfuric acid tower (12) from second stage sulfuric acid tower (13) sulfuric acid absorption liquid out;
F. the methyl chloride gas that obtains of described step e is after compressor (15) is compressed to 0.7MPa, enter water cooler (16) and carry out cooling and condensation obtains methyl chloride liquid product, finally enter liquid chlorine methane storage tank (17) storage.
CN201210326303.3A 2012-09-05 2012-09-05 Method for synthesizing chloromethane by tail gas generated during chloroacetic acid production Active CN102816045B (en)

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