CN106220469A - A kind of production and processing technology of 2,4 dichlorotoleune - Google Patents
A kind of production and processing technology of 2,4 dichlorotoleune Download PDFInfo
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- CN106220469A CN106220469A CN201610619322.3A CN201610619322A CN106220469A CN 106220469 A CN106220469 A CN 106220469A CN 201610619322 A CN201610619322 A CN 201610619322A CN 106220469 A CN106220469 A CN 106220469A
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- molecular sieve
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/08—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y
- B01J29/16—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J29/166—Y-type faujasite
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/093—Preparation of halogenated hydrocarbons by replacement by halogens
- C07C17/10—Preparation of halogenated hydrocarbons by replacement by halogens of hydrogen atoms
- C07C17/12—Preparation of halogenated hydrocarbons by replacement by halogens of hydrogen atoms in the ring of aromatic compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
- B01J2229/186—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself not in framework positions
Abstract
The present invention relates to a kind of 2, the production and processing technology of 4 dichlorotoleune, described synthesis technique is as follows: the 1) production of chlorination catalyst: with ReY type molecular sieve as carrier, ReY type molecular sieve is put into and carries out adsorbing and drying to iron chloride, zinc chloride, aluminum chloride, calcium chloride solution, can be prepared by chlorination catalyst；2) chlorination of parachlorotoluene: add parachlorotoluene in a kettle., and add chlorination catalyst in reactor, and be passed through chlorine, add alkaline solution in the mixture generated and react, and the waste residue produced in production process is reclaimed；3) component separates: by through step 2) after the mixture that generates carries out four rectification, and collect tower bottoms, i.e. can get 2,4 dichlorotoleune and 3,4 dichlorotoleune；The present invention is effectively improved the effect of chlorination catalyst, is effectively increased reaction rate and reaction yield, is effectively improved 2, the selectivity of 4 dichlorotoleune, it is suppressed that the generation of by-product, improves 2, the yield of 4 dichlorotoleune.
Description
Technical field
The invention belongs to technical field of organic chemistry, relate to the production and processing technology of a kind of 2,4-DCT.
Background technology
2,4-DCT is highly important organic synthesis fine-chemical intermediate, may be used for synthesizing 2,4-dichloro chlorine
Benzyl, 2,4-dichlorobenzaldehyde, 2,4-dichlorobenzoic acid, wait multiple Organic chemical products, be herbicide pyrazolate, antibacterial alkene azoles
The primary raw material of alcohol, medicine ciprofloxacin etc., and it is widely used in the industries such as pesticide, medicine, dyestuff, along with China Fine Chemical Industry
Development, the market demand of 2,4-DCT will increase day by day, and 2,4-DCT will have a good market prospect, and 2,4-
Dichlorotoleune is colourless transparent liquid, is important industrial chemicals, is mainly used in organic synthesis, pharmacy and dye industry, is also
A kind of good high boiling organic solvent, in current domestic and international existing synthesis technique, in production technology, production cost is high, technique
Complexity, product yield is low, and by-product is many, acid waste water is many, catalyst consumption amount big, therefore, how to produce a kind of work
Skill is simple, and the synthesis technique that product yield is high becomes numerous producer problem to be solved.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, it is provided that the production and processing technology of a kind of 2,4-DCT,
To solve problems of the prior art.
For achieving the above object, the technical solution used in the present invention is as follows:
The production and processing technology of a kind of 2,4-DCT, it is characterised in that described synthesis technique is as follows: 1) chlorination catalyst
Produce: with ReY type molecular sieve as carrier, ReY type molecular sieve is put into iron chloride, zinc chloride, aluminum chloride, calcium chloride solution
Adsorb, and carry out drying 4-6 hour at the ReY type molecular sieve after absorption is placed on 94-98 DEG C, can be prepared by chlorination
Catalyst；2) chlorination of parachlorotoluene: add parachlorotoluene in a kettle., and add chlorination catalyst in reactor, and
After making mixture carry out mix and blend 4-5 hour in batch mixing, in reactor, it is passed through chlorine and makes mixture at 35-39 DEG C
Under react, and make reaction stop after carrying out 14-18 hour being passed through chlorine, in reactor, be passed through nitrogen, and remove dress
Remaining chlorine and the hydrogen chloride gas of generation in putting, and the gas of generation is reclaimed, add in the mixture generated
Enter alkaline solution and react, and the waste residue produced in production process is reclaimed；3) component separates: will be through step 2)
After the mixture generated carries out a rectification in sending into the first rectifying column, the liquid of top of the tower after a rectification is sent into Second distillation column
Inside carry out secondary rectification, and collect tower bottoms, in the tower bottoms after secondary rectification is fed through the 3rd rectifying column, carry out three essences
Evaporate, and collect tower bottoms, after carrying out four rectification in the tower bottoms after three rectification is delivered to the 4th rectifying column, and collect tower reactor
Liquid, i.e. can get 2,4-DCT and 3,4-dichlorotoleune.
As a modification of the present invention, described step 2) in the mol ratio of parachlorotoluene and chlorine be 1:0.6-0.8.
As a modification of the present invention, described step 2) neutral and alkali solution is sodium hydroxide solution.
As a modification of the present invention, described step 2) in the weight ratio of chlorination catalyst and parachlorotoluene be 1:1.1-
1.5。
As a modification of the present invention, in described step 1), the production of chlorination catalyst comprises the following steps: (1) is by chlorine
Change ferrum, zinc chloride, aluminum chloride are stirred mixing with weight ratio for 8:5:1, and to make the pH value of solution be 1-2, by calcium chloride, chlorine
Change aluminum and be stirred mixing with weight ratio for 4:7, and to make the pH value of solution be 1-2, the aqueous solution that twice prepares is carried out respectively
Energising, and make mixture solution energising 5-7 hour；(2) with ReY type molecular sieve as carrier, ReY type molecular sieve is put into step
Suddenly in (1) in the mixed solution of the iron chloride of gained, zinc chloride, aluminum chloride, and ReY type molecular sieve is made to carry out at 68-72 DEG C
After soaking 3.5-5 hour, ReY type molecular sieve is put into step (1) calcium chloride of gained, the mixed solution of aluminum chloride
In, and make ReY type molecular sieve carry out soaking 4-5 hour at 82-85 DEG C；(3) will be through the ReY type after step (2) is soaked
Molecular sieve takes out, and carries out at ReY type molecular sieve is placed on 22-24 DEG C standing 4-5 days；(4) will be after step (3) stands
ReY type molecular sieve put into in the calcium chloride of step (1) gained, the mixed solution of aluminum chloride, and make ReY type molecular sieve
After carrying out soaking 4-6 hour at 87-95 DEG C, ReY type molecular sieve is taken out, and ReY type molecular sieve is put into step (1)
The iron chloride of middle gained, zinc chloride, aluminum chloride mixed solution in, and make ReY type molecular sieve carry out at 85-90 DEG C soak 4-
After 7 hours, ReY type molecular sieve is taken out；(5) the ReY type molecular sieve after taking out carries out placing 1-2 days at 26-30 DEG C
After, ReY type molecular sieve is placed on ventilation, and after making ReY type molecular sieve carry out placing 7-8 days at 20-23 DEG C, and will
ReY type molecular sieve carries out at being placed on 94-98 DEG C drying 4-6 hour, can be prepared by chlorination catalyst.
Owing to have employed above technology, the present invention compared with the prior art, has the advantage that as follows:
The present invention uses ReY type molecular sieve to be carrier, by the iron chloride after ReY type molecular sieve and electrolysis, zinc chloride, aluminum chloride
After acidic mixture mixes, then by the calcium chloride after ReY type molecular sieve and electrolysis, the acidic mixture of aluminum chloride mixes
Close, mixed ReY type molecular sieve is stood, iron chloride, zinc chloride, aluminum chloride, calcium chloride can be made preferably to adhere to
On ReY type molecular sieve, ReY type molecular sieve is mixed with the calcium chloride after electrolysis, the acidic mixture of aluminum chloride again
After, ReY type molecular sieve is mixed with the iron chloride after electrolysis, zinc chloride, the acidic mixture of aluminum chloride, will be through secondary
ReY type molecular sieve after immersion, and after being aerated drying, and carry out ReY type molecular sieve at 94-98 DEG C drying 4-6
Hour, iron chloride, zinc chloride, aluminum chloride, calcium chloride can be made preferably to be attached on ReY type molecular sieve, can be effectively improved
The effect of chlorination catalyst, is effectively increased reaction rate and reaction yield, is effectively improved the choosing to 2,4-DCT
Selecting property, owing to reaction temperature is relatively low, effectively inhibits the generation of the by-product such as benzotrichloride, toluene tetrachloride, improves 2,4-
The yield of dichlorotoleune, method is easy, easily operation, effective, and product yield is high；By mixture is carried out four times in the present invention
Rectification, can effectively remove the by-product produced in mixture, and successively the by-product of generation be carried out rectification and purification out, can
To be recycled by the by-product of generation, effectively prevent the waste of resource, the 2 of high yield can be obtained, 4-dichloromethane
Benzene.
Detailed description of the invention
Below in conjunction with detailed description of the invention, it is further elucidated with the present invention.
Embodiment 1:
The production and processing technology of a kind of 2,4-DCT, described synthesis technique is as follows: the 1) production of chlorination catalyst: with ReY
Type molecular sieve is carrier, is put into by ReY type molecular sieve and adsorbs to iron chloride, zinc chloride, aluminum chloride, calcium chloride solution,
And the ReY type molecular sieve after adsorbing is placed at 94 DEG C and carries out drying 4 hours, can be prepared by chlorination catalyst；2) to chlorine
The chlorination of toluene: add parachlorotoluene in a kettle., and add chlorination catalyst in reactor, and make mixture at batch mixing
In carry out mix and blend after 4 hours, in reactor, be passed through chlorine and make mixture react at 39 DEG C, and making reaction
Stop after carrying out 14 hours being passed through chlorine, in reactor, be passed through remaining chlorine and generation in nitrogen, and removing device
Hydrogen chloride gas, and the gas of generation is reclaimed, in the mixture generated, adds alkaline solution and react, and
The waste residue produced in production process is reclaimed；3) component separates: will be through step 2) mixture that generates sends into the first essence
After carrying out a rectification in evaporating tower, carry out secondary rectification in the liquid of top of the tower after a rectification is sent into Second distillation column, and collect
Tower bottoms, carries out three rectification in the tower bottoms after secondary rectification is fed through the 3rd rectifying column, and collects tower bottoms, by three times
After tower bottoms after rectification carries out four rectification in delivering to the 4th rectifying column, and collect tower bottoms, i.e. can get 2,4-dichloromethane
Benzene and 3,4-dichlorotoleune.
Described step 2) in the mol ratio of parachlorotoluene and chlorine be 1:0.6.
Described step 2) neutral and alkali solution is sodium hydroxide solution.
Described step 2) in the weight ratio of chlorination catalyst and parachlorotoluene be 1:1.5.
In described step 1), the production of chlorination catalyst comprises the following steps: (1) by iron chloride, zinc chloride, aluminum chloride with
Weight ratio is that 8:5:1 is stirred mixing, and to make the pH value of solution be 1, calcium chloride, aluminum chloride is carried out with weight ratio for 4:7
Stirring mixing, and to make the pH value of solution be 1, is energized respectively by the aqueous solution that twice prepares, and makes mixture solution energising 7
Individual hour；(2) with ReY type molecular sieve as carrier, ReY type molecular sieve is put into the iron chloride of gained, chlorination to step (1)
Zinc, aluminum chloride mixed solution in, and after making ReY type molecular sieve carry out soaking 3.5 hours at 72 DEG C, by ReY type molecule
Sieve is put into step (1) in the mixed solution of the calcium chloride of gained, aluminum chloride, and makes ReY type molecular sieve carry out at 82 DEG C
Soak 5 hours；(3) will take out through the ReY type molecular sieve after step (2) is soaked, and ReY type molecular sieve will be placed on 22 DEG C
Under carry out standing 5 days；(4) the ReY type molecular sieve after step (3) stands is put into the chlorination through step (1) gained
Calcium, aluminum chloride mixed solution in, and after making ReY type molecular sieve carry out soaking 6 hours at 87 DEG C, by ReY type molecular sieve
Take out, and ReY type molecular sieve is put into step (1) in the mixed solution of the iron chloride of gained, zinc chloride, aluminum chloride, and
After making ReY type molecular sieve carry out soaking 4 hours at 85 DEG C, ReY type molecular sieve is taken out；(5) the ReY type after taking out divides
After son sieve carries out placing 1 day at 30 DEG C, ReY type molecular sieve is placed on ventilation, and makes ReY type molecular sieve enter at 23 DEG C
Row was placed after 8 days, and was placed at 94 DEG C by ReY type molecular sieve and carries out drying 4 hours, can be prepared by chlorination catalyst.
After tested, product yield is 68.9%, and chlorine utilization is 97.2%, and in finished product, the purity of 2,4-DCT is
99.9%。
Embodiment 2:
The production and processing technology of a kind of 2,4-DCT, described synthesis technique is as follows: the 1) production of chlorination catalyst: with ReY
Type molecular sieve is carrier, is put into by ReY type molecular sieve and adsorbs to iron chloride, zinc chloride, aluminum chloride, calcium chloride solution,
And the ReY type molecular sieve after adsorbing is placed at 98 DEG C and carries out drying 4 hours, can be prepared by chlorination catalyst；2) to chlorine
The chlorination of toluene: add parachlorotoluene in a kettle., and add chlorination catalyst in reactor, and make mixture at batch mixing
In carry out mix and blend after 4 hours, in reactor, be passed through chlorine and make mixture react at 39 DEG C, and making reaction
Stop after carrying out 14 hours being passed through chlorine, in reactor, be passed through remaining chlorine and generation in nitrogen, and removing device
Hydrogen chloride gas, and the gas of generation is reclaimed, in the mixture generated, adds alkaline solution and react, and
The waste residue produced in production process is reclaimed；3) component separates: will be through step 2) mixture that generates sends into the first essence
After carrying out a rectification in evaporating tower, carry out secondary rectification in the liquid of top of the tower after a rectification is sent into Second distillation column, and collect
Tower bottoms, carries out three rectification in the tower bottoms after secondary rectification is fed through the 3rd rectifying column, and collects tower bottoms, by three times
After tower bottoms after rectification carries out four rectification in delivering to the 4th rectifying column, and collect tower bottoms, i.e. can get 2,4-dichloromethane
Benzene and 3,4-dichlorotoleune.
Described step 2) in the mol ratio of parachlorotoluene and chlorine be 10:8.
Described step 2) neutral and alkali solution is sodium hydroxide solution.
Described step 2) in the weight ratio of chlorination catalyst and parachlorotoluene be 1:1.5.
In described step 1), the production of chlorination catalyst comprises the following steps: (1) by iron chloride, zinc chloride, aluminum chloride with
Weight ratio is that 8:5:1 is stirred mixing, and to make the pH value of solution be 1, calcium chloride, aluminum chloride is carried out with weight ratio for 4:7
Stirring mixing, and to make the pH value of solution be 1, is energized respectively by the aqueous solution that twice prepares, and makes mixture solution energising 7
Individual hour；(2) with ReY type molecular sieve as carrier, ReY type molecular sieve is put into the iron chloride of gained, chlorination to step (1)
Zinc, aluminum chloride mixed solution in, and after making ReY type molecular sieve carry out soaking 4 hours at 68 DEG C, by ReY type molecular sieve
Put into step (1) in the mixed solution of the calcium chloride of gained, aluminum chloride, and make ReY type molecular sieve soak at 82 DEG C
Steep 5 hours；(3) will take out through the ReY type molecular sieve after step (2) is soaked, and ReY type molecular sieve will be placed at 23 DEG C
Carry out standing 4 days；(4) by through step (3) stand after ReY type molecular sieve put into through step (1) gained calcium chloride,
In the mixed solution of aluminum chloride, and after making ReY type molecular sieve carry out soaking 5 hours at 90 DEG C, ReY type molecular sieve is taken
Go out, and ReY type molecular sieve is put into step (1) in the mixed solution of the iron chloride of gained, zinc chloride, aluminum chloride, and make
ReY type molecular sieve is taken out after carrying out soaking 4 hours at 88 DEG C by ReY type molecular sieve；(5) the ReY type molecule after taking out
After sieve carries out placing 2 days at 26 DEG C, ReY type molecular sieve is placed on ventilation, and makes ReY type molecular sieve carry out at 20 DEG C
After placing 7 days, and ReY type molecular sieve is placed at 98 DEG C carries out drying 4 hours, can be prepared by chlorination catalyst.
After tested, product yield is 68.6%, and chlorine utilization is 96.9%, and in finished product, the purity of 2,4-DCT is
99.9%。
Embodiment 3:
The production and processing technology of a kind of 2,4-DCT, described synthesis technique is as follows: the 1) production of chlorination catalyst: with ReY
Type molecular sieve is carrier, is put into by ReY type molecular sieve and adsorbs to iron chloride, zinc chloride, aluminum chloride, calcium chloride solution,
And the ReY type molecular sieve after adsorbing is placed at 97 DEG C and carries out drying 5 hours, can be prepared by chlorination catalyst；2) to chlorine
The chlorination of toluene: add parachlorotoluene in a kettle., and add chlorination catalyst in reactor, and make mixture at batch mixing
In carry out mix and blend after 5 hours, in reactor, be passed through chlorine and make mixture react at 38 DEG C, and making reaction
Stop after carrying out 17 hours being passed through chlorine, in reactor, be passed through remaining chlorine and generation in nitrogen, and removing device
Hydrogen chloride gas, and the gas of generation is reclaimed, in the mixture generated, adds alkaline solution and react, and
The waste residue produced in production process is reclaimed；3) component separates: will be through step 2) mixture that generates sends into the first essence
After carrying out a rectification in evaporating tower, carry out secondary rectification in the liquid of top of the tower after a rectification is sent into Second distillation column, and collect
Tower bottoms, carries out three rectification in the tower bottoms after secondary rectification is fed through the 3rd rectifying column, and collects tower bottoms, by three times
After tower bottoms after rectification carries out four rectification in delivering to the 4th rectifying column, and collect tower bottoms, i.e. can get 2,4-dichloromethane
Benzene and 3,4-dichlorotoleune.
Described step 2) in the mol ratio of parachlorotoluene and chlorine be 1:0.7.
Described step 2) neutral and alkali solution is sodium hydroxide solution.
Described step 2) in the weight ratio of chlorination catalyst and parachlorotoluene be 1:1.3.
In described step 1), the production of chlorination catalyst comprises the following steps: (1) by iron chloride, zinc chloride, aluminum chloride with
Weight ratio is that 8:5:1 is stirred mixing, and to make the pH value of solution be 2, calcium chloride, aluminum chloride is carried out with weight ratio for 4:7
Stirring mixing, and to make the pH value of solution be 2, is energized respectively by the aqueous solution that twice prepares, and makes mixture solution energising 5
Individual hour；(2) with ReY type molecular sieve as carrier, ReY type molecular sieve is put into the iron chloride of gained, chlorination to step (1)
Zinc, aluminum chloride mixed solution in, and after making ReY type molecular sieve carry out soaking 4 hours at 70 DEG C, by ReY type molecular sieve
Put into step (1) in the mixed solution of the calcium chloride of gained, aluminum chloride, and make ReY type molecular sieve soak at 85 DEG C
Steep 4 hours；(3) will take out through the ReY type molecular sieve after step (2) is soaked, and ReY type molecular sieve will be placed at 23 DEG C
Carry out standing 4 days；(4) by through step (3) stand after ReY type molecular sieve put into through step (1) gained calcium chloride,
In the mixed solution of aluminum chloride, and after making ReY type molecular sieve carry out soaking 6 hours at 90 DEG C, ReY type molecular sieve is taken
Go out, and ReY type molecular sieve is put into step (1) in the mixed solution of the iron chloride of gained, zinc chloride, aluminum chloride, and make
ReY type molecular sieve is taken out after carrying out soaking 4 hours at 85 DEG C by ReY type molecular sieve；(5) the ReY type molecule after taking out
After sieve carries out placing 1 day at 29 DEG C, ReY type molecular sieve is placed on ventilation, and makes ReY type molecular sieve carry out at 22 DEG C
After placing 8 days, and ReY type molecular sieve is placed at 97 DEG C carries out drying 5 hours, can be prepared by chlorination catalyst.
After tested, product yield is 68.7%, and chlorine utilization is 97.1%, and in finished product, the purity of 2,4-DCT is
99.9%。
Above-described embodiment is only the preferred technical solution of the present invention, and is not construed as the restriction for the present invention, the present invention
Protection domain should with claim record technical scheme, including claim record technical scheme in technical characteristic etc.
Being protection domain with alternative, equivalent the most in this range is improved, also within protection scope of the present invention.
Claims (5)
1. the production and processing technology of a 2,4-DCT, it is characterised in that described synthesis technique is as follows: 1) chlorination catalyst
Production: with ReY type molecular sieve as carrier, ReY type molecular sieve is put into iron chloride, zinc chloride, aluminum chloride, calcium chloride solution
In adsorb, and carry out drying 4-6 hour at the ReY type molecular sieve after absorption is placed on 94-98 DEG C, can be prepared by chlorine
Change catalyst；2) chlorination of parachlorotoluene: add parachlorotoluene in a kettle., and add chlorination catalyst in reactor,
And after making mixture carry out mix and blend 4-5 hour in batch mixing, in reactor, be passed through chlorine and make mixture at 35-39
React at DEG C, and make reaction stop being passed through chlorine after carrying out 14-18 hour, in reactor, be passed through nitrogen, and remove
Remaining chlorine and the hydrogen chloride gas of generation in device, and the gas of generation is reclaimed, in the mixture generated
Add alkaline solution and react, and the waste residue produced in production process is reclaimed；3) component separates: will be through step
2), after the mixture generated carries out a rectification in sending into the first rectifying column, the liquid of top of the tower after a rectification is sent into the second rectification
Carry out secondary rectification in tower, and collect tower bottoms, in the tower bottoms after secondary rectification is fed through the 3rd rectifying column, carry out three times
Rectification, and collect tower bottoms, after carrying out four rectification in the tower bottoms after three rectification is delivered to the 4th rectifying column, and collect tower
Still liquid, i.e. can get 2,4-DCT and 3,4-dichlorotoleune.
The synthesis technique of a kind of 2,4-DCT the most according to claim 1, it is characterised in that: described step 2) in right
Chlorotoluene is 1:0.6-0.8 with the mol ratio of chlorine.
The synthesis technique of a kind of 2,4-DCT the most according to claim 1, it is characterised in that: described step 2) in alkali
Property solution is sodium hydroxide solution.
The synthesis technique of a kind of 2,4-DCT the most according to claim 1, it is characterised in that: described step 2) in chlorine
The weight ratio changing catalyst and parachlorotoluene is 1:1.1-1.5.
The synthesis technique of a kind of 2,4-DCT the most according to claim 1, it is characterised in that chlorine in described step 1)
The production changing catalyst comprises the following steps: iron chloride, zinc chloride, aluminum chloride are stirred mixing for 8:5:1 by (1) with weight ratio
Close, and to make the pH value of solution be 1-2, calcium chloride, aluminum chloride for 4:7, are stirred mixing with weight ratio, and make the pH of solution
Value is 1-2, is energized respectively by the aqueous solution that twice prepares, and makes mixture solution energising 5-7 hour；(2) with ReY type
Molecular sieve is carrier, and ReY type molecular sieve is put into step (1) iron chloride of gained, zinc chloride, the mixed solution of aluminum chloride
In, and after making ReY type molecular sieve carry out soaking 3.5-5 hour at 68-72 DEG C, ReY type molecular sieve is put into step (1)
The calcium chloride of middle gained, aluminum chloride mixed solution in, and it is little to make ReY type molecular sieve carry out soaking 4-5 at 82-85 DEG C
Time；(3) will take out through the ReY type molecular sieve after step (2) is soaked, and carry out at ReY type molecular sieve is placed on 22-24 DEG C
Stand 4-5 days；(4) the ReY type molecular sieve after step (3) stands is put into through the calcium chloride of step (1) gained, chlorine
Change in the mixed solution of aluminum, and after making ReY type molecular sieve carry out soaking 4-6 hour at 87-95 DEG C, by ReY type molecular sieve
Take out, and ReY type molecular sieve is put into step (1) in the mixed solution of the iron chloride of gained, zinc chloride, aluminum chloride, and
ReY type molecular sieve is made to be taken out by ReY type molecular sieve after carrying out soaking 4-7 hour at 85-90 DEG C；(5) ReY after taking out
After type molecular sieve carries out placing 1-2 days at 26-30 DEG C, ReY type molecular sieve is placed on ventilation, and makes ReY type molecular sieve
Carry out placing after 7-8 days at 20-23 DEG C, and carry out drying 4-6 hour at ReY type molecular sieve is placed on 94-98 DEG C, i.e.
Chlorination catalyst can be prepared.
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| CN108339555A (en) * | 2017-01-24 | 2018-07-31 | 盐城恒盛化工有限公司 | A kind of method of support type chlorination catalyst and preparation method thereof and synthesis 4 chloro pyridine |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108339555A (en) * | 2017-01-24 | 2018-07-31 | 盐城恒盛化工有限公司 | A kind of method of support type chlorination catalyst and preparation method thereof and synthesis 4 chloro pyridine |
| CN108339555B (en) * | 2017-01-24 | 2021-10-29 | 盐城恒盛化工有限公司 | Supported chlorination catalyst, preparation method thereof and method for synthesizing tetrachloropyridine |
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