CN109851490A - The chloroacetic technique of acetic anhydride catalyst method continuous production - Google Patents
The chloroacetic technique of acetic anhydride catalyst method continuous production Download PDFInfo
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Abstract
A kind of monoxone acetic anhydride catalysis continuity method new process, production stage are as follows: using acetic acid and chlorine as raw material, using aceticanhydride as catalyst, chlorine reaction is led in level-one chlorination reaction main still, reaction solution is transported to secondary chlorination reaction main still with pump；Continue logical chlorine reaction in secondary chlorination reaction main still, secondary chlorination is reacted into the reaction solution in main still with pump and is transported to hydrolysis kettle；Suitable water is added in hydrolysis kettle, the complete intermediate product of unreacted is removed by hydrolysis, the reaction solution pump after hydrolysis is transported to rectifying column；Steam is passed through to the reboiler of rectifying column to heat material, by reaction solution light component acetic acid and heavy constituent monoxone separate.The reaction gas of chlorinating containers at different levels condenses out the liquid foam carried secretly in reaction gas by I and II condenser, is returned in respective chlorinating container by reflux line, is sent to vent gas treatment process by the condensed reaction gas of condenser and is further processed.
Description
Technical field
The present invention relates to production of chloroacetic acid technologies, and in particular to the new process of monoxone acetic anhydride catalysis continuity method.
Background technique
Monoxone is produced using acetic acid and chlorine as raw material, chemical equation is as follows:
Produced in monoxone technique by raw material of glacial acetic acid and chlorine, according to catalyst used in reacting it is different and
Whether process continuously derives a variety of different production technologies.Wherein, by the catalyst difference used be divided into sulfur catalyst method and
Two kinds of acetic anhydride catalyst method, batch process and two kinds of continuity method are divided into whether by production process continuously.Country's monoxone industry is raw at present
Producing chloroacetic technique mainly has 3 kinds of production works such as sulphur catalysis batch process, acetic anhydride catalysis batch process, acetic anhydride catalysis continuity method
Skill, and mostly based on sulphur catalysis batch process production technology, the disadvantage is that containing in major product monoxone and byproduct hydrochloric acid
There is elemental sulfur and its compound to cause its of poor quality, byproduct hydrochloric acid because contain elemental sulfur and its subsequent use of compounds affect,
Purification difficulty is big, at high cost.The country also has part monoxone device to produce using acetic anhydride catalysis batch process, major product chloroethene
Acid and byproduct hydrochloric acid quality increase, but due to being produced using one-pot batch process, and installation area is big, the degree of automation
It is low.The investment construction first set acetic anhydride catalysis continuity method monoxone life at home at first of beginning of this century Akzo Nobel N.V., Holland
Device is produced, which produces monoxone using acetic anhydride catalysis continuous chlorination, but because its technical barrier is stern, invests the originals such as big
Cause, which is not yet received at home is widely applied.
Sulphur is catalyzed chloroacetic acid by intermittent process production technology, is to produce using acetic acid and chlorine as raw material by catalyst of sulphur
Monoxone, major defect are as follows:
1. sulphur is catalyzed chloroacetic acid by intermittent process production technology, using one-pot batch production, the phase is with a chlorine after the reaction
When acetic acid concentration reaches 90% or more, the side reaction for generating dichloroacetic acid is gradually increased, and dichloroacetic acid in final products is caused to contain
It measures higher, has certain influence to product quality.
2. leading to product monoxone containing elemental sulfur and its compound in chloroethene acid product due to using sulphur as catalyst
Impurity is more, influences downstream use.
3. because causing byproduct hydrochloric acid of poor quality containing the compounds such as elemental sulfur and sulfuric acid, sulfurous acid in byproduct hydrochloric acid,
And purification difficulty is big, at high cost, downstream is difficult to be utilized, and environmentally friendly hidden danger is larger.
4. installation area is big, the degree of automation is low.
The country also has part monoxone device to produce using acetic anhydride catalysis batch process, major product monoxone and byproduct hydrochloric acid
Quality increases, but due to being produced using one-pot batch process, installation area is big, the degree of automation is low.
Summary of the invention
In view of the above-mentioned problems, the present invention is using acetic acid and chlorine as raw material, using aceticanhydride as catalyst, using continuous production processes
Monoxone is produced, and monoxone is subjected to rectification and purification, major product monoxone and byproduct hydrochloric acid quality is made to be largely increased
Chloroacetic acid producing process.
New process overcomes the shortcomings that acetic anhydride catalysis batch process, takes the method for continuous chlorination and mentions in conjunction with monoxone rectifying
Production processes of chloroacetic acid is divided into two parts of chlorination reaction and rectification and purification, both can achieve the mesh of continuous chlorination by pure technology
, and product quality can be improved, and substantially reduce investment outlay than international continuity method process units.
Present invention aim to provide a kind of new monoxone continuity method production technology, keep production of chloroacetic acid continuous
It carries out, realizes automation convenient for device.
Realization of the invention, comprising the following steps:
1) using acetic acid and chlorine as raw material, using aceticanhydride as catalyst, lead to chlorine in level-one chlorination reaction main still and be reacted to a chlorine
When acetic acid concentration reaches 70~75%%, reaction solution is transported to secondary chlorination reaction main still with pump；
2) it in secondary chlorination reaction main still, reaction solution is continued logical chlorine is reacted to chloroacetic acid concentration to reach 85-90%
After terminate chlorination reaction, with pump by secondary chlorination react main still in reaction solution be transported to hydrolysis kettle；
3) suitable water is added in hydrolysis kettle, the complete intermediate product of unreacted is removed by hydrolysis, and will pass through
Reaction solution pump after hydrolysis is transported to rectifying column；
4) steam is passed through into reboiler collet to heat material, material is made to reach fluidized state, it will be therein light
Component steams, and boil-off gas condenses out chloroacetic acid by the packing layer and first-stage condenser of rectifying column, returns to rectifying column bottom
Portion；
5) boil-off gas continues through secondary condenser and further condenses out light component (main component is acetic acid), collects
It is stored into light component tank, and continuously sends chlorination reaction process back to pump and recycle；Rectifier bottoms material is by essence
The chloroethene acid product for evaporating purification is stored with product storage tank is pumped into.
6) reaction gas of level-one chlorination reaction main still condenses the liquid foam carried secretly in reaction gas by one, secondary condenser
Get off, is returned in level-one chlorination reaction main still by reflux line to reduce reaction mass loss；
7) reaction gas of secondary chlorination reaction main still condenses the liquid foam carried secretly in reaction gas by one, secondary condenser
Get off, secondary chlorination is returned to by reflux line and is reacted in main still；
8) enter chlorination after collecting from the reaction gas that level-one main still secondary condenser and second level main still secondary condenser come out
Secondary kettle is reacted, remaining chlorine continues in reaction gas and acetic acid reaction is to reduce the free chlorine contents in tail gas；
9) reaction gas come out from chlorination reaction pair kettle will be reacted by secondary kettle first-stage condenser and secondary kettle secondary condenser
The liquid foam carried secretly in gas, which condenses out and passes through reflux line, returns to chlorination reaction pair kettle, comes out from secondary kettle secondary condenser anti-
Should gas be pipelined to vent gas treatment process and be further processed.
Above-mentioned chlorination reaction liquid chloroacetic acid concentration in level-one chlorination reaction main still controls between 70~75%.
Above-mentioned chlorination reaction liquid reaction temperature in level-one chlorination reaction main still controls between 95~105 DEG C.
Above-mentioned chlorination reaction liquid chloroacetic acid concentration in secondary chlorination reaction main still controls between 85~90%.
Above-mentioned chlorination reaction liquid reaction temperature in secondary chlorination reaction main still controls between 95~105 DEG C.
Above-mentioned chlorination reaction liquid is in temperature control in hydrolysis kettle between 105~115 DEG C.
Above-mentioned chlorination reaction liquid is in water content control in hydrolysis kettle between 0.5~1.0%.
Above-mentioned chlorination reaction liquid controls between 130~140 DEG C in rectifying column bottom temperature.
Above-mentioned chlorination reaction liquid controls between 100~110 DEG C in rectifying tower top temperature.
Technical solution of the present invention provides a kind of new monoxone continuity method process units under conditions of above-mentioned technique, makes
Production of chloroacetic acid can be carried out continuously, and realize automation convenient for device.
A kind of continuous production device for chloroacetic acid, including chlorination reaction pair kettle, level-one chlorination reaction main still, secondary chlorination are anti-
Answer main still, level-one main still first-stage condenser, level-one main still secondary condenser, second level main still first-stage condenser, second level main still second level
Condenser, secondary kettle first-stage condenser, secondary kettle secondary condenser, hydrolysis kettle, rectifying column, reboiler, rectifying first-stage condenser, rectifying
Secondary condenser, light component tank；
Chlorination reaction pair kettle outlet at bottom connects level-one chlorination reaction main still upper inlet, level-one chlorine by delivery pump pipeline
Change reaction main still outlet at bottom and secondary chlorination reaction main still upper inlet is connected by delivery pump pipeline, secondary chlorination reacts main still
Bottom end outlet connects hydrolysis kettle upper inlet by delivery pump pipeline, and hydrolysis kettle bottom end outlet connects rectifying by delivery pump pipeline
The feed inlet of tower, rectifier bottoms are connected to monoxone product storage tank.
Rectifier bottoms are connected with reboiler, and reboiler is connected by circulation to rectifying column.
The top of rectifying column is connected with the bottom of rectifying first-stage condenser, the top of rectifying first-stage condenser by pipeline with
The top of rectifying secondary condenser is connected, and the bottom of rectifying secondary condenser is connected with light component tank.
The top gas phase outlet of level-one chlorination reaction main still is connected with the lower part of level-one main still first-stage condenser, level-one main still
The top gas phase outlet of first-stage condenser is connected with the lower part of level-one main still secondary condenser, level-one main still secondary condenser bottom
It is connect with level-one chlorination reaction main still, the top gas phase outlet of level-one main still secondary condenser is connect with chlorination reaction pair kettle.
The top gas phase outlet of the secondary chlorination reaction main still is connected with the lower part of second level main still first-stage condenser, and two
The top gas phase outlet of grade main still first-stage condenser is connected with the lower part of second level main still secondary condenser, second level main still B-grade condensation
Device bottom is connect with secondary chlorination reaction main still, is connect at the top of second level main still secondary condenser with chlorination reaction pair kettle.
The upper gaseous phase outlet of the chlorination reaction pair kettle is connected with the bottom of secondary kettle first-stage condenser, and secondary kettle level-one is cold
The top gas phase outlet of condenser is connected with the lower part of secondary kettle secondary condenser, and the top gas phase of secondary kettle secondary condenser exports connection
Vent gas treatment process.
A kind of monoxone acetic anhydride catalysis continuity method new process, using acetic acid and chlorine as raw material, using aceticanhydride as catalyst, respectively
When being reacted to chloroacetic acid concentration by continuous chlorination in I and II chlorinating container and reaching 85~90%, by reaction solution into
Rectifying column, which is sent to, after row hydrolysis carries out rectification and purification.Its advantage is as follows:
1. traditional sulphur is catalyzed chloroacetic acid by intermittent process production technology, chlorination reaction is divided into three early period, mid-term, later period ranks
Section, the phase, chloroacetic acid continued the pair of chlorination generation dichloroacetic acid with chloroacetic acid concentration raising (reaching 90%) after the reaction
Reaction can gradually increase, and cause to react a large amount of dichloroacetic acid of later period generation, keep dichloroacetic acid content in final products higher, shadow
Ring monoxone product quality.New process controls chloroacetic acid maximum concentration in reaction solution and is no more than 90%, avoids later period chlorination
Excessive dichloroacetic acid is generated in reaction process, is reduced the chance of dichloroacetic acid generation, is contained the dichloroacetic acid in reaction solution
Amount is greatly reduced, and product quality significantly improves.
2. using aceticanhydride as catalyst, since aceticanhydride is the product after acetic acid shrinks, in reaction solution without introduce impurity at
Point, chloroethene acid product improves monoxone product purity without impurity such as elemental sulfur and sulfide.
3. using aceticanhydride as catalyst, in the hydrochloric acid of chlorination reaction by-product not the compound impurities such as sulfur acid, sulfurous acid at
Point, byproduct hydrochloric acid quality greatly improves, and is conducive to downstream and uses, environmental protection pressure reduces.
4. new process introduces rectifying and purifying system, by light group of the complete acetic acid of unreacted in reaction solution and reaction intermediate etc.
Divide and separated from product, keeps monoxone product purity higher.
5. the monoxone product quality of traditional sulphur catalysis batch process production are as follows: chloroacetic acid content 93~94%, dichloro
Acetic acid content 4.5~5.0%；The monoxone product quality of acetic anhydride catalysis continuity method new process production are as follows: chloroacetic acid content
96.0~96.5%, dichloroacetic acid content 2.0~2.5%, it is seen that new process monoxone product quality is largely increased.
6. using continuity method production technology, raw material input and output of products are all made of the mode being carried out continuously, and are conducive to
Device realizes automation control, greatly improves plant automation level.
7. external acetic anhydride catalysis continuity method process units process flow is long, installation area is big, investment is big, and a set of 60,000
Ton/year monoxone plant investment about between 1.8~2.0 hundred million yuan；The continuity method process units process flow of this acetic anhydride catalysis
It is short, installation area is small, with low investment, a set of 60,000 tons/year of monoxone plant investment about between 0.8~1.0 hundred million yuan, dress
It sets investment and saves nearly half.
Detailed description of the invention
Fig. 1 is continuous production device for chloroacetic acid structure chart, wherein 1. chlorination reaction pair kettles 1,2. level-one chlorination reaction masters
Kettle, 3. secondary chlorinations reaction main still, 4. hydrolysis kettles, 5. secondary kettle first-stage condensers, 6. secondary kettle secondary condensers, 7. level-one main stills one
Grade condenser, 8. level-one main still secondary condensers, 9. second level main still first-stage condensers, 10. second level main still secondary condensers, 11.
Rectifying column, 12. rectifying first-stage condensers, 13. rectifying secondary condensers, 14. light component tanks, 15. reboilers.
Specific embodiment
Embodiment 1
1) using acetic acid and chlorine as raw material, using aceticanhydride as catalyst, feed liquid temperature is controlled in level-one chlorination reaction main still
At 98 DEG C, logical chlorine reaction makes chloroacetic acid concentration in reaction solution reach 73%, and reaction solution is transported to secondary chlorination reaction with pump
Main still；
2) in secondary chlorination reaction main still, keep feed liquid temperature at 97 DEG C, continuing logical chlorine makes chloroacetic acid in reaction solution
Concentration terminates chlorination reaction when reaching 88%, and secondary chlorination is reacted the reaction solution in main still with pump and is transported to hydrolysis kettle；
3) reacting liquid temperature in hydrolysis kettle is increased to 110 DEG C, suitable water is added in hydrolysis kettle, controls and contains in reaction solution
Water is removed 0.8%, by the complete intermediate product of unreacted by hydrolysis, and the reaction solution pump after hydrolysis is defeated
It is sent to rectifying column；
4) it is passed through steam into reboiler collet to heat material, reaction solution is controlled in rectifying column bottom temperature 135
DEG C, tower top temperature control is 105 DEG C, and the light component in reaction solution is steamed, and boil-off gas passes through the packing layer and level-one of rectifying column
Condenser condenses out chloroacetic acid, returns to rectifier bottoms；
5) boil-off gas continues through secondary condenser and further condenses out light component (main component is acetic acid), collects
It is stored into light component tank, and continuously sends chlorination reaction process back to pump and recycle；Rectifier bottoms material is by essence
The chloroethene acid product for evaporating purification is stored with product storage tank is pumped into.
6) reaction gas of chlorination reaction main stills at different levels will be under the liquid foam that carried secretly in reaction gas condensation by I and II condenser
Come, the control of rectifying first-stage condenser gaseous phase outlet temperature is 80 DEG C, and the control of rectifying secondary condenser gaseous phase outlet temperature is 25 DEG C；
It is returned in respective chlorination reaction main still by reflux line；The reaction gas come out from the secondary condenser of I and II main still collects
Enter chlorination reaction pair kettle afterwards, remaining chlorine continues in secondary kettle and is pipelined to tail after acetic acid reaction in reaction gas
Gas disposal process is further processed.
The monoxone product quality of acetic anhydride catalysis continuity method new process production are as follows: chloroacetic acid content 96.3%, two chloroethenes
Acid content 2.5%.
Embodiment 2
1) using acetic acid and chlorine as raw material, using aceticanhydride as catalyst, feed liquid temperature is controlled in level-one chlorination reaction main still
At 97 DEG C, logical chlorine reaction makes chloroacetic acid concentration in reaction solution reach 71%, and reaction solution is transported to secondary chlorination reaction with pump
Main still；
2) in secondary chlorination reaction main still, keep feed liquid temperature at 99 DEG C, continuing logical chlorine makes chloroacetic acid in reaction solution
Concentration terminates chlorination reaction when reaching 87%, and secondary chlorination is reacted the reaction solution in main still with pump and is transported to hydrolysis kettle；
3) reacting liquid temperature in hydrolysis kettle is increased to 112 DEG C, suitable water is added in hydrolysis kettle, controls and contains in reaction solution
Water is removed 0.7%, by the complete intermediate product of unreacted by hydrolysis, and the reaction solution pump after hydrolysis is defeated
It is sent to rectifying column；
4) it is passed through steam into reboiler collet to heat material, reaction solution is controlled in rectifying column bottom temperature 137
DEG C, tower top temperature control is 110 DEG C, and the light component in reaction solution is steamed, and boil-off gas passes through the packing layer and level-one of rectifying column
Condenser condenses out chloroacetic acid, returns to rectifier bottoms；
5) boil-off gas continues through secondary condenser and further condenses out light component (main component is acetic acid), collects
It is stored into light component tank, and continuously sends chlorination reaction process back to pump and recycle；Rectifier bottoms material is by essence
The chloroethene acid product for evaporating purification is stored with product storage tank is pumped into.
6) reaction gas of chlorination reaction main stills at different levels will be under the liquid foam that carried secretly in reaction gas condensation by I and II condenser
Come, the control of rectifying first-stage condenser gaseous phase outlet temperature is 85 DEG C, and the control of rectifying secondary condenser gaseous phase outlet temperature is 30 DEG C；
It is returned in respective chlorination reaction main still by reflux line；The reaction gas come out from the secondary condenser of I and II main still collects
Enter chlorination reaction pair kettle afterwards, remaining chlorine continues in secondary kettle and is pipelined to tail after acetic acid reaction in reaction gas
Gas disposal process is further processed.
The monoxone product quality of acetic anhydride catalysis continuity method new process production are as follows: chloroacetic acid content 96.4%, two chloroethenes
Acid content 2.45%.
Embodiment 3
1) using acetic acid and chlorine as raw material, using aceticanhydride as catalyst, feed liquid temperature is controlled in level-one chlorination reaction main still
At 100 DEG C, logical chlorine reaction makes chloroacetic acid concentration in reaction solution reach 74%, and reaction solution is transported to secondary chlorination reaction with pump
Main still；
2) in secondary chlorination reaction main still, keep feed liquid temperature at 102 DEG C, continuing logical chlorine makes chloroacetic acid in reaction solution
Concentration terminates chlorination reaction when reaching 89%, and secondary chlorination is reacted the reaction solution in main still with pump and is transported to hydrolysis kettle；
3) reacting liquid temperature in hydrolysis kettle is increased to 114 DEG C, suitable water is added in hydrolysis kettle, controls and contains in reaction solution
Water is removed 0.9%, by the complete intermediate product of unreacted by hydrolysis, and the reaction solution pump after hydrolysis is defeated
It is sent to rectifying column；
4) it is passed through steam into reboiler collet to heat material, reaction solution is controlled in rectifying column bottom temperature 133
DEG C, tower top temperature control is 100 DEG C, and the light component in reaction solution is steamed, and boil-off gas passes through the packing layer and level-one of rectifying column
Condenser condenses out chloroacetic acid, returns to rectifier bottoms；
5) boil-off gas continues through secondary condenser and further condenses out light component (main component is acetic acid), collects
It is stored into light component tank, and continuously sends chlorination reaction process back to pump and recycle；Rectifier bottoms material is by essence
The chloroethene acid product for evaporating purification is stored with product storage tank is pumped into.
6) reaction gas of chlorination reaction main stills at different levels will be under the liquid foam that carried secretly in reaction gas condensation by I and II condenser
Come, the control of rectifying first-stage condenser gaseous phase outlet temperature is 75 DEG C, and the control of rectifying secondary condenser gaseous phase outlet temperature is 28 DEG C；
It is returned in respective chlorination reaction main still by reflux line；The reaction gas come out from the secondary condenser of I and II main still collects
Enter chlorination reaction pair kettle afterwards, remaining chlorine continues in secondary kettle and is pipelined to tail after acetic acid reaction in reaction gas
Gas disposal process is further processed.
The monoxone product quality of acetic anhydride catalysis continuity method new process production are as follows: chloroacetic acid content 96.5%, two chloroethenes
Acid content 2.5%.
Embodiment 4
The reaction gas of level-one chlorination reaction main still passes through level-one main still first-stage condenser and level-one main still secondary condenser will
The liquid foam carried secretly in reaction gas condenses out, and is returned in level-one chlorination reaction main still by reflux line.Secondary chlorination reaction master
The reaction gas of kettle condenses the liquid foam carried secretly in reaction gas by second level main still first-stage condenser and second level main still secondary condenser
Get off, secondary chlorination is returned to by reflux line and is reacted in main still.It is cold from level-one main still secondary condenser and second level main still second level
The reaction gas that condenser comes out enters chlorination reaction pair kettle after collecting, remaining chlorine continues in reaction gas and acetic acid reaction is to reduce
Free chlorine contents in tail gas.The reaction gas come out from chlorination reaction pair kettle, it is cold by secondary kettle first-stage condenser and secondary kettle second level
Condenser condenses out the liquid foam carried secretly in reaction gas, and is returned in chlorination reaction pair kettle by reflux line.From secondary kettle second level
The reaction gas that condenser comes out is pipelined to vent gas treatment process and is further processed.
Specific device structure is a kind of continuous production device for chloroacetic acid, including chlorination reaction pair kettle 1, level-one chlorination reaction
Main still 2, secondary chlorination react main still 3, level-one main still first-stage condenser 7, level-one main still secondary condenser 8, second level main still level-one
Condenser 9, second level main still secondary condenser 10, secondary kettle first-stage condenser 5, secondary kettle secondary condenser 6, hydrolysis kettle 4, rectifying column
11, reboiler 15, rectifying first-stage condenser 12, rectifying secondary condenser 13, light component tank 14；
1 outlet at bottom of chlorination reaction pair kettle connects 2 upper inlet of level-one chlorination reaction main still, level-one by delivery pump pipeline
2 outlet at bottom of chlorination reaction main still connects secondary chlorination by delivery pump pipeline and reacts 3 upper inlet of main still, secondary chlorination reaction
3 bottom end outlet of main still connects 4 upper inlet of hydrolysis kettle by delivery pump pipeline, and 4 bottom end outlet of hydrolysis kettle passes through delivery pump pipeline
The feed inlet of rectifying column 11 is connected, 11 bottom of rectifying column is connected to monoxone product storage tank.
11 bottom of rectifying column is connected with reboiler 15, and reboiler 15 is connected by circulation to rectifying column 11.
The top of rectifying column 11 is connected with the bottom of rectifying first-stage condenser 12, and the top of rectifying first-stage condenser 12 passes through
Pipeline is connected with the top of rectifying secondary condenser 13, and the bottom of rectifying secondary condenser 13 is connected with light component tank 14.
The top gas phase outlet of level-one chlorination reaction main still 2 is connected with the lower part of level-one main still first-stage condenser 7, level-one master
The top gas phase outlet of kettle first-stage condenser 7 is connected with the lower part of level-one main still secondary condenser 8, level-one main still secondary condenser
8 bottoms are connect with level-one chlorination reaction main still 2, top gas phase outlet and the chlorination reaction pair kettle 1 of level-one main still secondary condenser 8
Connection.
The top gas phase outlet of secondary chlorination reaction main still 3 is connected with the lower part of second level main still first-stage condenser 9, second level master
The top gas phase outlet of kettle first-stage condenser 9 is connected with the lower part of second level main still secondary condenser 10, second level main still B-grade condensation
10 bottom of device is connect with secondary chlorination reaction main still 3, and 10 top of second level main still secondary condenser is connect with chlorination reaction pair kettle 1.
The upper gaseous phase outlet of chlorination reaction pair kettle 1 is connected with the bottom of secondary kettle first-stage condenser 5, secondary kettle first-stage condenser
5 top gas phase outlet is connected with the lower part of secondary kettle secondary condenser 6, and the top gas phase of secondary kettle secondary condenser 6 exports connection
Vent gas treatment process.
Claims (7)
1. the chloroacetic technique of acetic anhydride catalyst method continuous production produces chlorine by catalyst of aceticanhydride using acetic acid and chlorine as raw material
Acetic acid, and monoxone is subjected to rectification and purification, it is characterized in that, comprising the following steps:
(1) using acetic acid and chlorine as raw material, using aceticanhydride as catalyst, one is reacted to after leading to chlorine in level-one chlorination reaction main still
When chloroethene acid concentration reaches 70~75%, reaction solution is transported to secondary chlorination reaction main still；
(2) in secondary chlorination reaction main still, reaction solution is continued into logical chlorine and is reacted to after chloroacetic acid concentration reaches 85~90% eventually
Secondary chlorination is reacted the reaction solution in main still and is transported to hydrolysis kettle by only chlorination reaction；
(3) suitable water is added in hydrolysis kettle, the complete intermediate product of unreacted is removed by hydrolysis, and will be by hydrolysis
Reaction solution pump afterwards is transported to rectifying column；
(4) steam is passed through into the reboiler collet of rectifying column to heat material, material is made to reach fluidized state, it will wherein
Light component steam, boil-off gas by rectifying column packing layer and first-stage condenser chloroacetic acid is condensed out, return to rectifying
Tower bottom；
(5) boil-off gas continues through secondary condenser and further condenses out light component, is collected into light component tank and stores, and
Chlorination reaction process is continuously sent back to pump to recycle；Rectifier bottoms material is the chloroethene acid product for passing through rectification and purification,
It is stored with product storage tank is pumped into.
2. the chloroacetic technique of acetic anhydride catalyst method continuous production according to claim 1, which is characterized in that level-one chlorination is anti-
The reaction gas of main still is answered to condense out the liquid foam carried secretly in reaction gas by its first-stage condenser, secondary condenser, by returning
Flow tube road returns in level-one chlorination reaction main still to reduce reaction mass loss；
The reaction gas of secondary chlorination reaction main still condenses out the liquid foam carried secretly in reaction gas by one, secondary condenser,
Secondary chlorination is returned to by reflux line to react in main still.
3. the chloroacetic technique of acetic anhydride catalyst method continuous production according to claim 1, which is characterized in that above-mentioned chlorination is anti-
Liquid reaction temperature in level-one chlorination reaction main still is answered to control between 95~105 DEG C.
4. the chloroacetic technique of acetic anhydride catalyst method continuous production according to claim 1, which is characterized in that above-mentioned chlorination is anti-
Liquid reaction temperature in secondary chlorination reaction main still is answered to control between 95~105 DEG C.
5. the chloroacetic technique of acetic anhydride catalyst method continuous production according to claim 1, which is characterized in that above-mentioned chlorination is anti-
Answer liquid in temperature control in hydrolysis kettle between 105~115 DEG C.
6. the chloroacetic technique of acetic anhydride catalyst method continuous production according to claim 1, which is characterized in that above-mentioned chlorination is anti-
Answer liquid in water content control in hydrolysis kettle between 0.5~1.0%.
7. the chloroacetic technique of acetic anhydride catalyst method continuous production according to claim 1, which is characterized in that above-mentioned chlorination is anti-
Answer liquid in the control of rectifying column bottom temperature between 130~140 DEG C；Above-mentioned chlorination reaction liquid is controlled in rectifying tower top temperature 100
Between~110 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114671772A (en) * | 2022-05-02 | 2022-06-28 | 闫三朋 | Production process of aminoacetic acid |
| CN115245792A (en) * | 2022-09-22 | 2022-10-28 | 山东民基新材料科技有限公司 | Chloroacetic acid synthesis system and synthesis method |
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