CN105218299B - Continuous preparation method for producing chlorohydrocarbon from carbon tetrachloride and olefin - Google Patents
Continuous preparation method for producing chlorohydrocarbon from carbon tetrachloride and olefin Download PDFInfo
- Publication number
- CN105218299B CN105218299B CN201510640252.5A CN201510640252A CN105218299B CN 105218299 B CN105218299 B CN 105218299B CN 201510640252 A CN201510640252 A CN 201510640252A CN 105218299 B CN105218299 B CN 105218299B
- Authority
- CN
- China
- Prior art keywords
- reaction
- chlorohydrocarbon
- carbon tetrachloride
- olefin
- kettle
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a continuous preparation method for producing chlorohydrocarbon by carbon tetrachloride and olefin, which comprises the following steps: (1) continuously adding iron powder or iron filler, catalyst auxiliary agent alkyl phosphate and carbon tetrachloride into a first ferrous complex catalyst preparation kettle; (2) conveying the material reacted in the step (1) to a second chlorohydrocarbon synthesis reaction kettle after quickly passing through a filter, and reacting with olefin continuously introduced into the chlorohydrocarbon synthesis reaction kettle; (3) and (3) introducing the crude halohydrocarbon obtained in the step (2) into a subsequent separation system, purifying and collecting the final target halohydrocarbon product. The invention separates the preparation of ferrous complex catalyst from the synthesis of chlorohydrocarbon, and avoids the reduction of catalytic activity of olefin self-polymer due to the adhesion of iron powder or iron filler. The method has simple process, further improves the reaction efficiency by controlling the temperature, time, pressure and the like of the reaction, and simultaneously ensures that the reaction product has higher yield and better selectivity.
Description
Technical Field
The invention relates to a continuous preparation method for producing chlorinated hydrocarbon by carbon tetrachloride and olefin.
Background
The structural formula in the art is CCl3CH2The current patent reports about the preparation method of chlorohydrocarbon (such as 1,1,1,3, 3-pentachloropropane) of CHnClm (n is 0-2, m is 3-n) mainly adopt two processes of batch reaction preparation and continuous reaction preparation, and a cuprous chloride complex catalytic system and an iron catalytic system are respectively adopted in the catalytic system. When the intermittent reaction is adopted to prepare the chlorohydrocarbon, the production efficiency is low, and the method is not suitable for industrial mass production of products. One obvious drawback encountered with cuprous chloride complex catalyst systems is that the cuprous complex catalyst cannot be recycled, since the catalyst and catalyst promoter are removed by washing with water, which completely destroys the catalyst, as described in patent CN1544403A, when recovering the chlorinated product. In addition, the cuprous chloride catalyst system is adopted, so that the corrosion to equipment and pipeline valves made of common stainless steel materials is high, and the requirement on production equipment is high.
Different from a cuprous chloride catalytic system, the iron catalyst has the advantages that the catalyst and the catalyst auxiliary agent can be recycled, and the requirement on equipment pipelines is not high due to the weak acidity of a reaction system. Therefore, the iron-based continuous catalytic telomerization reaction is adopted, so that the reaction efficiency is greatly improved compared with that of an intermittent reaction, the production cost is effectively reduced, the three wastes are reduced, the requirement on the material of equipment and pipelines is not high, and the common stainless steel can be used for a longer time. However, most of the patents report that when the chlorohydrocarbons (such as chlorohydrocarbon (HCC240fa)) are synthesized by continuous reaction using an iron catalyst system, the influence of olefin self-polymerization byproducts on the reaction is avoided. During the telomerization and addition reaction of carbon tetrachloride and olefin, small amount of olefin polymerization reaction may occur simultaneously. When the accumulation of the olefin self-polymerization in the reaction kettle becomes large for a long time, the olefin self-polymerization can wrap the iron powder or the iron filler, so that the iron powder or the iron filler is adhered and agglomerated with each other, and the activity of the iron powder or the iron filler is very adversely affected. In addition, the iron powder or iron filler wrappage is not easy to be removed when being stuck on the kettle wall or the stirring paddle, which causes destructive influence on the production continuity.
Disclosure of Invention
The invention aims to provide a technical scheme for a continuous preparation method for producing chlorohydrocarbon by carbon tetrachloride and olefin aiming at the defects in the prior art, the original reaction design is changed, the continuous preparation method is disassembled into two reaction components, iron powder or iron filler in the reaction is blocked in a first reaction kettle by a filter and cannot be contacted with a byproduct olefin self-polymer in a second reaction kettle, the phenomenon of mutual adhesion and agglomeration among the iron powder or iron filler is effectively avoided, the activity of the iron powder or iron filler is improved, the reaction effect is better, the loss of energy consumption is reduced, and the comprehensive utilization rate is improved.
In order to solve the technical problems, the technical scheme adopted by the invention is a continuous preparation method for producing chlorinated hydrocarbon by carbon tetrachloride and olefin, which is characterized by comprising the following steps:
(1) continuously adding iron powder or iron filler, catalyst auxiliary agent alkyl phosphate and carbon tetrachloride into a first ferrous complex catalyst preparation kettle, wherein the reaction temperature is 90-130 ℃, the reaction pressure is 0.1-0.3 MPa, and the reaction residence time is 0.3-2 h.
(2) Filtering the materials reacted in the step (1) by a filter quickly to remove iron powder or iron filler, conveying the materials to a second chlorohydrocarbon synthesis reaction kettle, and reacting the materials with olefin continuously introduced into the chlorohydrocarbon synthesis reaction kettle to generate a crude product containing a target product halohydrocarbon, wherein the reaction temperature is 90-130 ℃, the reaction pressure is 0.1-0.5 MPa, and the reaction residence time is 0.5-2 hours.
(3) And (3) introducing the crude halohydrocarbon obtained in the step (2) into a subsequent separation system, recycling unreacted materials, catalysts and catalyst auxiliaries, purifying and collecting a final target halohydrocarbon product, firstly carrying out flash evaporation to remove unreacted carbon tetrachloride, olefin and chlorohydrocarbon product components, introducing a flash evaporation liquid into a primary rectifying tower, rectifying and recovering unreacted carbon tetrachloride and olefin, circularly returning the carbon tetrachloride and olefin to the chlorohydrocarbon synthesis reaction kettle in the step (2), introducing the material containing the target chlorohydrocarbon product left in the primary rectifying tower into a secondary rectifying tower for purifying and collecting the target product, wherein flash evaporation residue contains iron or ferrous ion alkyl phosphate complex or alkyl phosphate, discharging from the bottom of a flash evaporation device, and circularly returning the material to a ferrous complex catalyst preparation kettle for reuse.
Further, chlorohydrocarbons were synthesized by telomerization of 1,1,1,3, 3-pentachloropropane (chlorohydrocarbon (HCC240fa)), 1,1,1,3,3, 3-hexachloropropane (HCC230fa), and 1,1,1, 3-tetrachloropropane (HCC250 fa).
Further, in the step (2), the olefin includes ethylene, monochloroethylene and vinylidene chloride.
Further, the iron filler comprises iron materials, such as iron rings, iron wires, scrap iron, stainless steel, carbon steel and the like, so that the iron filler is easy to obtain, and the cost is reduced.
Furthermore, the catalyst promoter is selected from one or more than one of alkyl phosphate esters such as triethyl phosphate, tributyl phosphate, trimethyl phosphate, triphenyl phosphate and the like, and the reaction efficiency is accelerated by using the catalyst promoter.
Further, the mass ratio of carbon tetrachloride to olefin is 1-10: 1, and the mass percentage of the catalyst promoter in the carbon tetrachloride is 1-5%; the iron powder or iron filler accounts for 0.1-1% of the total mass of the mixed material, and the reaction effect is better, the yield of the product after reaction is higher, and the selectivity is better through the control of the proportion.
Further, in the step (1), the reaction temperature is preferably 95-120 ℃, the reaction residence time is preferably 0.3-1.5 h, and by controlling the reaction temperature and the reaction time, the reaction of the materials in the step (1) is more complete and sufficient, the waste of resources is reduced, and the high efficiency of the reaction is ensured.
Further, in the step (2), the reaction temperature is preferably 95-120 ℃, the reaction residence time is preferably 0.5-1.5 h, the reaction pressure is related to the amount of the introduced olefin and the activity of the catalyst, generally 0.15-0.5 Mpa, and the reaction temperature in the step (2) is controlled, so that the reaction efficiency can be improved, the reaction time can be controlled, the incomplete reaction caused by too short reaction time can be avoided, the raw material residue can be caused, the conversion rate is low, the reaction time can be prevented from being too long, byproducts can be generated, and the product selectivity can be reduced.
Furthermore, the distance between the ferrous complex catalyst preparation kettle and the chlorohydrocarbon synthesis reaction kettle is less than 2 meters, heat preservation measures are made on the pipeline, the conveying retention time of the discharged reaction materials on the pipeline between the two reaction kettles is shortened by shortening the pipeline distance of the two reaction kettles or increasing the pipe diameter, the reaction effect is improved, meanwhile, the design of the heat preservation measures can ensure the temperature of the materials in conveying, and the phenomenon that due to the large temperature difference, part of active free radicals generated in the ferrous complex catalyst preparation kettle are quenched is avoided.
Further, in the step (2), the filter is a filter cloth or a ceramic membrane, and iron powder or iron filler is filtered by the filter, so that the adverse effect of separation caused by the fact that the iron powder or iron filler enters a subsequent rectification system is avoided.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
1. through the design of the ferrous complex catalyst preparation kettle and the chlorohydrocarbon synthesis reaction kettle, the reaction is decomposed into two reactions, so that the phenomenon that iron powder and iron filler are adhered and agglomerated in each other in the reaction process is effectively avoided, and the production efficiency is improved;
2. the method has simple process, and further improves the reaction rate by controlling the temperature, time, pressure and the like of the reaction, so that the yield of the reaction product is higher and the selectivity is better;
3. the waste utilization rate is high, the production cost is reduced, and the waste of resources is avoided;
4. the generated chlorohydrocarbon product has good selectivity and high quality, and can realize industrial continuous production due to easy feeding.
Because the iron powder or the iron filler is blocked in the preparation kettle of the ferrous complex catalyst by the filter, the iron powder or the iron filler cannot contact with a small amount of olefin self-polymer generated in the reaction of the second chlorohydrocarbon synthesis reaction kettle, so that the reduction of the activity and the utilization rate of the iron powder or the iron filler due to the wrapping of the olefin self-polymer is avoided, the iron powder or the iron filler is prevented from being adhered to the kettle wall or a stirring blade and difficult to remove, and the reaction rate is improved.
Drawings
The invention will be further described with reference to the accompanying drawings in which:
FIG. 1 is a schematic diagram of a continuous synthesis process for chlorohydrocarbon (HCC240fa) according to the present invention;
FIG. 2 is a comparative process flow diagram for the synthesis of chlorinated hydrocarbons (HCC240fa) according to the invention.
In the figure: a-a ferrous complex catalyst preparation kettle; b-a reaction kettle for synthesizing chlorinated hydrocarbon; c-a flash distillation unit; d-a first-stage rectifying tower; e-a secondary rectification column; f. g-filter.
Detailed Description
The invention relates to a continuous preparation method for producing chlorohydrocarbon by carbon tetrachloride and olefin, which comprises the following steps:
(1) continuously adding iron powder or iron filler, catalyst auxiliaries, namely alkyl phosphate and carbon tetrachloride into a first ferrous complex catalyst preparation kettle, wherein the iron filler comprises iron materials, such as iron rings, iron wires, scrap iron, even various iron-containing substances such as stainless steel and carbon steel, so that the iron filler is easier to obtain, the cost is reduced, the catalyst auxiliaries are selected from one or more than one of alkyl phosphate esters such as triethyl phosphate, tributyl phosphate, trimethyl phosphate and triphenyl phosphate, the reaction efficiency is accelerated by using the catalyst auxiliaries, the mass ratio of the carbon tetrachloride to the olefin is 1-10: 1, and the catalyst auxiliaries account for 1-5% by mass of the carbon tetrachloride; the iron powder or iron filler accounts for 0.1-1% of the total mass of the mixed material, the reaction effect is better through proportion control, the yield of the product after reaction is higher, the selectivity is better, the reaction temperature is 90-130 ℃, the reaction pressure is 0.1-0.3 MPa, the reaction residence time is 0.3-2 h, the reaction temperature is preferably 95-120 ℃, the reaction residence time is preferably 0.3-1.5 h, the reaction temperature and the reaction time are controlled, so that the reaction of the material in the step (1) is more complete and sufficient, the waste of resources is reduced, and the high efficiency of the reaction is ensured.
(2) Filtering iron powder or iron filler from the material reacted in the step (1) through a filter quickly, conveying the material to a second chlorohydrocarbon synthesis reaction kettle, reacting the material with olefin continuously introduced into the chlorohydrocarbon synthesis reaction kettle to generate a crude product containing a target product, wherein the filter is a filter cloth or ceramic membrane, filtering the iron powder or iron filler through the filter to avoid the adverse effect of separation of the iron powder or iron filler in a subsequent rectification system, the olefin comprises ethylene, monochloroethylene and vinylidene chloride, the reaction temperature is 90-130 ℃, the reaction pressure is 0.1-0.5 MPa, the reaction residence time is 0.5-2 h, the reaction temperature is preferably 95-120 ℃, the reaction residence time is preferably 0.5-1.5 h, the reaction pressure is related to the amount of the introduced olefin and the activity of a catalyst, and is generally 0.15-0.5 MPa, and controlling the reaction temperature in the step (2) can improve the reaction efficiency, the reaction time is controlled, so that the reaction incomplete caused by too short reaction time and raw material residue caused by incomplete reaction can be avoided, the conversion rate is low, and the by-products generated by too long reaction time and the reduction of product selectivity can be prevented.
(3) Introducing the crude halohydrocarbon obtained in the step (2) into a subsequent separation system, recycling unreacted materials, catalysts and catalyst auxiliaries, purifying and collecting a final target halohydrocarbon product, firstly carrying out flash evaporation to remove unreacted carbon tetrachloride, olefin and chlorohydrocarbon product components, introducing flash evaporation liquid into a primary rectifying tower, rectifying and recovering unreacted carbon tetrachloride and olefin, and circularly returning the carbon tetrachloride and olefin to the chlorohydrocarbon synthesis reaction kettle in the step (2), introducing the material containing the target chlorohydrocarbon product remained in the primary rectifying tower into a secondary rectifying tower for purifying and collecting the target product, wherein flash evaporation residue contains iron or ferrous ion-containing alkyl phosphate complex or alkyl phosphate, discharging from the bottom of a flash evaporation device and circularly returning the material to a ferrous complex catalyst preparation kettle for reuse, and the distance between the ferrous complex catalyst preparation kettle and the chlorohydrocarbon synthesis reaction kettle is less than 2m, and heat preservation measures are made on the pipeline, the conveying retention time of the discharged reaction materials on the pipeline between the two reaction kettles is shortened by shortening the pipeline distance of the two reaction kettles or increasing the pipe diameter, the reaction effect is improved, and meanwhile, the design of the heat preservation measures can ensure the temperature of the materials in the conveying process, and the phenomenon that due to the large temperature difference, part of active free radicals generated in the ferrous complex catalyst preparation kettle are quenched is avoided.
Example 1
As shown in fig. 1
Mixing carbon tetrachloride, iron powder (80 meshes) and triethyl phosphate, conveying the mixture into a 100L ferrous complex catalyst preparation kettle by a slurry pump, wherein the reaction temperature in the kettle is 100 ℃, the reaction pressure is 0.15MPa, the reaction residence time is 1h, the reacted material mixture is quickly conveyed into a second 100L chlorohydrocarbon synthesis reaction kettle by a filter, the distance between the two kettles is 1.5m, the inner diameter of a conveying pipe is 75mm, Vinyl Chloride (VCM) is introduced into the chlorohydrocarbon synthesis reaction kettle from the lower part to perform telomerization reaction with the carbon tetrachloride, the mass ratio of the carbon tetrachloride, the vinyl chloride and the triethyl phosphate is 70:14:1, the iron powder accounts for 0.1 wt% of the mixed material, the reaction temperature is 100 ℃, the reaction pressure is 0.2MPa, and the reaction residence time is 1h,
the reaction product flows through a film evaporator for flash evaporation, light components such as carbon tetrachloride, chloroethylene and chlorohydrocarbon (HCC240fa) enter a primary rectifying tower, unreacted carbon tetrachloride and chloroethylene are extracted from the top of the tower and circularly returned to a chlorohydrocarbon synthesis reaction kettle, the tower bottom liquid enters a secondary rectifying tower to obtain a chlorohydrocarbon (HCC240fa) pure product, and flash evaporation residual liquid contains ferrous/ferric ion complex and triethyl phosphate and circularly returns to a ferrous complex catalyst preparation kettle from the bottom of the flash evaporation tower for reuse.
In this example, after 4 days of operation, the average conversion rate of vinyl chloride is 98.4%, the average selectivity of chlorohydrocarbon (HCC240fa) is 98.2%, the purity is more than 99.0%, and no iron powder adhesive is found on the wall and the stirring paddle when the chlorohydrocarbon synthesis reaction kettle is opened.
Example 2
As shown in fig. 2
Mixing carbon tetrachloride, iron powder (80 meshes) and triethyl phosphate, conveying the mixture into a 100L chlorohydrocarbon synthesis reaction kettle through a slurry pump, introducing chloroethylene into the chlorohydrocarbon synthesis reaction kettle from the lower part of the reactor to perform telomerization reaction with the carbon tetrachloride, wherein the mass ratio of the carbon tetrachloride to the chloroethylene to the triethyl phosphate is 70:14:1, the iron powder accounts for 0.1 wt% of the mixture, the reaction temperature is 100 ℃, the reaction pressure is 0.2MPa, and the reaction residence time is 1 h.
Removing iron powder from a reaction product by a filter, sending the reaction product into a film evaporator for flash evaporation, enabling light components such as carbon tetrachloride, chloroethylene and chlorohydrocarbon (HCC240fa) to enter a primary rectifying tower, extracting unreacted carbon tetrachloride and chloroethylene from the top of the tower, circularly returning the carbon tetrachloride and chloroethylene to a chlorohydrocarbon synthesis reaction kettle, enabling tower bottom liquid to enter a secondary rectifying tower to obtain a chlorohydrocarbon (HCC240fa) pure product, and enabling flash evaporation residual liquid to contain ferrous/iron ion complex and triethyl phosphate to be circularly returned to the chlorohydrocarbon synthesis reaction kettle from the bottom of the flash evaporation tower for reuse.
The operation of the embodiment is carried out for 4 days, the average conversion rate of the chloroethylene is 98.2%, the average selectivity of the chlorohydrocarbon (HCC240fa) is 98.0%, the purity is more than 99.0%, the chlorohydrocarbon synthesis reaction kettle is opened to clean iron powder sticky on the kettle wall and the stirring paddle, 10Kg of chloroethylene self-polymer is obtained by drying and weighing, and 0.2Kg of chloroethylene self-polymer is obtained by washing and drying hydrochloric acid for removing iron.
Comparative example 3
Mixing carbon tetrachloride, iron powder (80 meshes) and tributyl phosphate, conveying the mixture to a 100L ferrous complex catalyst preparation kettle through a slurry pump, wherein the reaction temperature in the kettle is 120 ℃, the reaction pressure is 0.2MPa, the reaction residence time is 0.5h, the reacted material mixture is quickly conveyed to a second 100L chlorohydrocarbon synthesis reaction kettle through a filter, the distance between the two kettles is 1.5m, the inner diameter of a conveying pipe is 75mm, vinyl chloride is introduced into the chlorohydrocarbon synthesis reaction kettle from the lower part to perform telomerization reaction with the carbon tetrachloride, the mass ratio of the carbon tetrachloride, the vinyl chloride and the tributyl phosphate is 70:28:1, the iron powder accounts for 0.2 wt% of the mixed material, the reaction temperature is 100 ℃, the reaction pressure is 0.3MPa, and the reaction residence time is 1.5 h.
The reaction product flows through a film evaporator for flash evaporation, light components such as carbon tetrachloride, chloroethylene and chlorohydrocarbon (HCC240fa) enter a primary rectifying tower, unreacted carbon tetrachloride and chloroethylene are extracted from the top of the tower and circularly returned to a chlorohydrocarbon synthesis reaction kettle, the tower bottom liquid enters a secondary rectifying tower to obtain a chlorohydrocarbon (HCC240fa) pure product, and flash evaporation residual liquid is directly discharged and is not recycled.
In the example, after running for 4 days, the average conversion rate of the vinyl chloride is 98.0 percent, the average selectivity of the chlorohydrocarbon (HCC240fa) is 98.0 percent, the purity is more than 99.0 percent, and iron powder sticky substances are hardly found on the kettle wall and the stirring paddle after the kettle of the chlorohydrocarbon synthesis reaction kettle is opened.
The above is only a specific embodiment of the present invention, but the technical features of the present invention are not limited thereto. Any simple variations, equivalent substitutions or modifications based on the present invention to achieve substantially the same technical effects are within the scope of the present invention.
Claims (3)
1. A continuous preparation method for producing chlorinated hydrocarbon by carbon tetrachloride and olefin is characterized by comprising the following steps:
(1) continuously adding iron powder, catalyst auxiliary agent alkyl phosphate and carbon tetrachloride into a first ferrous complex catalyst preparation kettle, wherein the reaction temperature is 90-130 ℃, the reaction pressure is 0.1-0.3 MPa, and the reaction residence time is 0.3-2 h; the catalyst auxiliary agent is selected from one or a mixture of more than one of triethyl phosphate and tributyl phosphate;
(2) filtering iron powder of the material reacted in the step (1) through a filter, conveying the material to a second chlorohydrocarbon synthesis reaction kettle, and reacting the material with olefin continuously introduced into the chlorohydrocarbon synthesis reaction kettle to generate a crude product containing a target product halohydrocarbon, wherein the olefin is monochloroethylene, the reaction temperature is 90-130 ℃, the reaction pressure is 0.1-0.5 MPa, and the reaction residence time is 0.5-2 h; the filter is filter cloth or a ceramic membrane;
(3) introducing the halogenated hydrocarbon crude product obtained in the step (2) into a subsequent separation system, recycling unreacted materials, catalyst and cocatalyst, purifying and collecting a final target halogenated hydrocarbon product, firstly performing flash evaporation to remove unreacted carbon tetrachloride, olefin and chlorinated hydrocarbon product components, introducing a flash evaporation liquid into a primary rectifying tower, rectifying and recovering unreacted carbon tetrachloride and olefin, wherein the mass ratio of the carbon tetrachloride to the olefin is 1-10: 1, and the catalyst auxiliary agent accounts for 1-5% of the carbon tetrachloride; the iron powder accounts for 0.1-1% of the total mass of the mixed materials and circularly returns to the chlorohydrocarbon synthesis reaction kettle in the step (2), the material containing the target chlorohydrocarbon product left in the primary rectifying tower is introduced into the secondary rectifying tower to be purified and collected with the target product, the flash distillation residue contains iron or ferrous ion alkyl phosphate complex or alkyl phosphate, the material is discharged from the bottom of the flash distillation device and circularly returns to the ferrous complex catalyst preparation kettle for reuse, and the distance between the ferrous complex catalyst preparation kettle and the chlorohydrocarbon synthesis reaction kettle is less than 2 meters; the chlorinated hydrocarbons consist of 1,1,1,3, 3-pentachloropropane (HCC240fa), 1,1,1,3,3, 3-hexachloropropane (HCC230fa), and 1,1,1, 3-tetrachloropropane (HCC250 fa).
2. A continuous process for the production of chlorinated hydrocarbons from carbon tetrachloride and olefins according to claim 1, characterized in that: in the step (1), the reaction temperature is 95-120 ℃, and the reaction residence time is 0.3-1.5 h.
3. A continuous process for the production of chlorinated hydrocarbons from carbon tetrachloride and olefins according to claim 1, characterized in that: in the step (2), the reaction temperature is 95-120 ℃, the reaction residence time is 0.5-1.5 h, and the reaction pressure is 0.15-0.5 MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510640252.5A CN105218299B (en) | 2015-09-30 | 2015-09-30 | Continuous preparation method for producing chlorohydrocarbon from carbon tetrachloride and olefin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510640252.5A CN105218299B (en) | 2015-09-30 | 2015-09-30 | Continuous preparation method for producing chlorohydrocarbon from carbon tetrachloride and olefin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105218299A CN105218299A (en) | 2016-01-06 |
| CN105218299B true CN105218299B (en) | 2020-03-31 |
Family
ID=54987648
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510640252.5A Active CN105218299B (en) | 2015-09-30 | 2015-09-30 | Continuous preparation method for producing chlorohydrocarbon from carbon tetrachloride and olefin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105218299B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018022488A1 (en) * | 2016-07-26 | 2018-02-01 | Occidental Chemical Corporation | Methods for producing halogenated propanes |
| CN109796300B (en) * | 2018-12-29 | 2020-12-18 | 浙江巨化技术中心有限公司 | Continuous preparation method of 2,3,3, 3-tetrafluoropropene |
| CN111659322A (en) * | 2019-03-06 | 2020-09-15 | 浙江佳汇新材料有限公司 | Device and process for preparing 1,1,1, 3-tetrachloropropane |
| CN112057929B (en) * | 2020-09-07 | 2022-05-31 | 江苏九九久科技有限公司 | Method for automatically separating and recycling solid catalyst in liquid reaction |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101558031A (en) * | 2006-10-11 | 2009-10-14 | 霍尼韦尔国际公司 | Process for the manufacture of 1,1,1,3,3-pentachloropropane |
| CN102056876A (en) * | 2008-04-09 | 2011-05-11 | 墨西哥化学阿玛科股份有限公司 | Process |
| CN103524291A (en) * | 2013-09-18 | 2014-01-22 | 巨化集团技术中心 | Continuous synthetic method of chloralkane |
-
2015
- 2015-09-30 CN CN201510640252.5A patent/CN105218299B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101558031A (en) * | 2006-10-11 | 2009-10-14 | 霍尼韦尔国际公司 | Process for the manufacture of 1,1,1,3,3-pentachloropropane |
| CN102056876A (en) * | 2008-04-09 | 2011-05-11 | 墨西哥化学阿玛科股份有限公司 | Process |
| CN103524291A (en) * | 2013-09-18 | 2014-01-22 | 巨化集团技术中心 | Continuous synthetic method of chloralkane |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105218299A (en) | 2016-01-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105218299B (en) | Continuous preparation method for producing chlorohydrocarbon from carbon tetrachloride and olefin | |
| JP6333939B2 (en) | Method for reducing by-product formation during the production of haloalkane compounds | |
| WO2012081482A1 (en) | Method for producing c3 chlorinated hydrocarbon | |
| US8722946B2 (en) | Method for avoiding the generation of by-products during the production of haloalkane compounds | |
| CN105026346A (en) | Synthesis of 1,1,2,3-tetrachloropropene | |
| CN111056913A (en) | Continuous production method of 1, 1, 1, 3-tetrachloropropane | |
| JP2017127870A (en) | Method for capturing and recycling iron catalyst used in production of haloalkane compound | |
| CN100427442C (en) | Improved preparing process for 1,1,1,3,3-pentachloro propane | |
| EP2840062A1 (en) | Method for utilizing fluoroalkyl iodide | |
| CN100406417C (en) | Method for preparing 1,1,1,3,3 - pentachlorobutane from materials of chloropropene and carbon tetrachloride under tempering and polymerizing catalyst | |
| US10017436B1 (en) | Method of making 1,1,1,2,3-pentachloropropane | |
| CN101786947B (en) | Method for preparing benzaldehyde by oxidizing toluene | |
| CN106146247A (en) | A kind of continuity method prepares the process of 1,1,1,3-tetra-chloropropane | |
| CN105622330A (en) | Continuous preparation method of chlorohydrocarbons | |
| CN110950735A (en) | Method for preparing 1,1,1,4,4, 4-hexafluoro-2-butyne by gas phase method | |
| CN114835564B (en) | Method for producing photoinitiator UV-1173 by condensation method | |
| CN107337576B (en) | Normal temperature catalytic synthesis of 2-bromo-5-fluorobenzotrifluoride | |
| CN103524291A (en) | Continuous synthetic method of chloralkane | |
| CN103524296A (en) | Preparation method of 1,1,2,3-tetrachloropropene | |
| CN107793384B (en) | Method for preparing 2, 5-dimethoxy-2, 5-dihydrofuran | |
| CN110950757B (en) | Production method and system of malonic diester | |
| CN215712715U (en) | Device for preparing 4-chlorophthalic anhydride | |
| CN108640821A (en) | A kind of the rubigan tertbutyl ether synthetic method and device of high-efficiency and continuous | |
| CN109608302B (en) | Preparation method of 2,3,3, 3-tetrafluoropropene | |
| CN111559952A (en) | Method for producing 1,1, 3-trichloropropene by liquid-phase dehydrochlorination of 1,1,1, 3-tetrachloropropane and catalyst recovery |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |