CN106669757A - Method for preparing catalyst of vinylidene chloride by gas phase catalytic cracking - Google Patents
Method for preparing catalyst of vinylidene chloride by gas phase catalytic cracking Download PDFInfo
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- CN106669757A CN106669757A CN201611196697.XA CN201611196697A CN106669757A CN 106669757 A CN106669757 A CN 106669757A CN 201611196697 A CN201611196697 A CN 201611196697A CN 106669757 A CN106669757 A CN 106669757A
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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Abstract
The invention discloses a method for preparing a catalyst of vinylidene chloride by gas phase catalytic cracking, comprising the following steps: step 1, adding a certain amount of dicyandiamide white powder into a certain proportion of pure water, carrying out magnetic stirring in a constant-temperature water bath; step 2, adding a certain proportion of liquid nano silicon dioxide into the solution obtained in the step 1; step 3, loading white gel of dicyandiamide and silicon dioxide obtained in the step 2 into a pipe furnace, heating from 20 DEG C to a certain temperature at a definite heating rate under nitrogen gas atmosphere, and keeping the constant-temperature state at the temperature; step 4, grinding a straw yellow product obtained in the step 3, and dispersing in an HF solution to obtain a C3N4 carbon nitrogen material catalyst; and step 5, loading the catalyst into a tube cracking furnace in which 1,1,2-trichloroethane performs gas phase dehydrochlorination reaction under the action of the catalyst to generate vinylidene chloride. The prepared catalyst has high activity and good stability.
Description
Technical field
The present invention relates to catalyst field, and in particular to for a kind of for preparing vinylidene chloride by gas-phase catalytic cracking
The method of catalyst.
Background technology
Vinylidene chloride（VDC）Monomer is a kind of critically important Organic Chemicals, and application is extensive.Vinylidene chloride
It is highly important Elementary Chemical Industry raw material in Polymers Synthesizing Technology, is the principal monomer for producing PVDC resins and PVDC latexes,
It is also the primary raw material for producing fluorochlorohydrocarbon succedaneum.Therefore, vinylidene chloride has wide market application foreground, greatly develops
Vinylidene chloride production technology is significant.
The traditional processing technology of vinylidene chloride is vinyl trichloride saponification method, because of its process is simple, investment relatively
It is less, for a long time both at home and abroad vinylidene chloride is produced in this way.But the method can produce a large amount of salt-containing organic wastewaters, not be inconsistent
Thus, vinyl trichloride prepares the range request excessively of vinylidene chloride and must develop new process route cyclization guaranteed request.
Vinyl trichloride gas phase catalysis cracking process prepares vinylidene chloride technique because its is pollution-free, low energy consumption, receives significant attention.
And 1,1,2- trichloroethane gas phase catalysis cracking processs prepare vinylidene chloride technique key be catalyst exploitation.
Patent No. US 4816609 propose by the use of alkali metal, the chloride of alkaline-earth metal or and mixture as catalyst,
The reaction of 1,1,2- trichloroethanes Gas phase dehydrochlorination is studied.
Patent No. US 3870762 proposes urging used in reaction 1,1,2- trichloroethane Gas phase dehydrochlorination courses of reaction
Agent mainly has potassium chloride, Rubinorm (Ifi)., cesium chloride, potassium fluoride etc..
But, above-mentioned catalyst it is active relatively low, and be easier to lose activity.
The content of the invention
It is an object of the invention to provide a kind of method of the catalyst for preparing vinylidene chloride by gas-phase catalytic cracking, with
Overcome existing technical problem.
The technical scheme is that：A kind of method of the catalyst for preparing vinylidene chloride by gas-phase catalytic cracking,
Comprise the following steps：
Step 1：A certain amount of dicyanodiamine white powder is added in a certain proportion of pure water, magnetic force is stirred in water bath with thermostatic control
Mix, be completely dissolved dicyanodiamine；
Step 2：A certain proportion of liquid nano silicon dioxide is added in the solution that step 1 is obtained, obtain dicyanodiamine with
The white gels of silicon dioxide；
Step 3：During the white gels material that step 2 is obtained is as tube furnace, in a nitrogen atmosphere by 20 DEG C with certain liter
Warm speed rises to uniform temperature, and keeps temperature constant state at this temperature, is cooled to after room temperature and obtains faint yellow product；
Step 4：The faint yellow product grinding that step 3 is obtained, and be stirred after being scattered in HF solution, then deionized water
Washed and drying with dehydrated alcohol, obtained C3N4Carbon-nitrogen material catalyst；
Step 5：By C3N4Carbon-nitrogen material catalyst is placed in tube cracking furnace, and vinyl trichloride is in C3N4Carbon-nitrogen material is urged
Gas phase dehydrochlorination reaction is carried out under agent effect, reaction generates vinylidene chloride.
Further, the temperature of the constant temperature water bath in the step 1 is 40-60 DEG C, a length of 15min during magnetic agitation.
Further, the heating rate in the step 3 is 5-20 DEG C/min.
Further, the temperature for rising in the step 3 is 400-600 DEG C.
Further, volume ratio of the nitrogen atmosphere in the step 3 comprising a certain amount of oxygen, oxygen and nitrogen is controlled
In 0%-5%.
Further, the deionized water and dehydrated alcohol in the step 4 is respectively washed 2-3 time, and it is little that 2 are dried at 50 DEG C
When.
Further, at 260 DEG C, air speed control exists the cracking reaction temperature control of the tube cracking furnace in the step 5
10min-1。
Further, the liquid nano silicon dioxide is controlled in 5-10 with the mass ratio of dicyanodiamine.
Beneficial effects of the present invention are：Jing after catalyst reaction in product inclined two vinyl chloride content, calculate not
Conversion ratio and selection of the catalyst prepared under same sintering temperature, different heating rates and different oxygen content to inclined two vinyl chloride
Property, from data in table, the activity of the catalyst of the preparation method preparation of the present invention is high, good stability, in addition, ring of the present invention
Protect pollution-free.
Specific embodiment
In order to deepen the understanding of the present invention, below in conjunction with embodiment, the invention will be further described, the embodiment
It is only used for explaining the present invention, does not constitute the restriction to protection scope of the present invention.
The technical scheme that the present invention is adopted, comprises the following steps：
Step 1：A certain amount of dicyanodiamine white powder is added in a certain proportion of pure water, in 40-60 DEG C of thermostatted water
Magnetic agitation 15min in bath, is completely dissolved dicyanodiamine；
Step 2：A certain proportion of liquid nano silicon dioxide is added in the solution that step 1 is obtained, obtain dicyanodiamine with
The white gels of silicon dioxide, wherein, liquid nano silicon dioxide is controlled in 5-10 with the mass ratio of dicyanodiamine；
Embodiment 1
The spawn obtained by step 1 and 2 is placed in tube furnace, by 20 DEG C of liters with 10 DEG C/min under pure nitrogen gas atmosphere
Warm speed rises to 400 DEG C, and constant temperature 5 hours at this temperature, is cooled to after room temperature and obtains faint yellow product, is ground to powder
After be scattered in HF solution, stir 10 hours, then respectively washing 3 times of deionized water and dehydrated alcohol, 2 are then dried at 50 DEG C
Hour, obtain C3N4Carbon-nitrogen material catalyst.
Obtained catalyst is placed in tube cracking furnace, vinyl trichloride carries out gas phase under catalyst action and takes off
Hcl reaction, reaction generates the products such as vinylidene chloride, 1,2-dichloroethene, hydrogen chloride.Cracking reaction temperature control is 260
DEG C, air speed is controlled in 10min-1。
Embodiment 2
The spawn obtained by step 1 and 2 is placed in tube furnace, by 20 DEG C of liters with 10 DEG C/min under pure nitrogen gas atmosphere
Warm speed rises to 550 DEG C, and constant temperature 5 hours at this temperature, is cooled to after room temperature and obtains faint yellow product, is ground to powder
After be scattered in HF solution, stir 10 hours, then respectively washing 3 times of deionized water and dehydrated alcohol, 2 are then dried at 50 DEG C
Hour, obtain C3N4Carbon-nitrogen material catalyst.
Obtained catalyst is placed in tube cracking furnace, vinyl trichloride carries out gas phase under catalyst action and takes off
Hcl reaction, reaction generates the products such as vinylidene chloride, 1,2-dichloroethene, hydrogen chloride.Cracking reaction temperature control is 260
DEG C, air speed is controlled in 10min-1。
Embodiment 3
The spawn obtained by step 1 and 2 is placed in tube furnace, by 20 DEG C of liters with 10 DEG C/min under pure nitrogen gas atmosphere
Warm speed rises to 600 DEG C, and constant temperature 5 hours at this temperature, is cooled to after room temperature and obtains faint yellow product, is ground to powder
After be scattered in HF solution, stir 10 hours, then respectively washing 3 times of deionized water and dehydrated alcohol, 2 are then dried at 50 DEG C
Hour, obtain C3N4Carbon-nitrogen material catalyst.
Obtained catalyst is placed in tube cracking furnace, vinyl trichloride carries out gas phase under catalyst action and takes off
Hcl reaction, reaction generates the products such as vinylidene chloride, 1,2-dichloroethene, hydrogen chloride.Cracking reaction temperature control is 260
DEG C, air speed is controlled in 10min-1。
Table 1 is that the catalyst prepared under different sintering temperatures affects on the selectivity of vinylidene chloride, and Jing catalyst is urged
Change the content of inclined two vinyl chloride in product after reaction, so as to calculate the conversion ratio and selectivity of inclined two vinyl chloride.
Table 1
Embodiment 4
The spawn obtained by step 1 and 2 is placed in tube furnace, by 20 DEG C of liters with 5 DEG C/min under pure nitrogen gas atmosphere
Warm speed rises to 550 DEG C, and constant temperature 5 hours at this temperature, is cooled to after room temperature and obtains faint yellow product, is ground to powder
After be scattered in HF solution, stir 10 hours, then respectively washing 3 times of deionized water and dehydrated alcohol, 2 are then dried at 50 DEG C
Hour, obtain C3N4Carbon-nitrogen material catalyst.
Obtained catalyst is placed in tube cracking furnace, vinyl trichloride carries out gas phase under catalyst action and takes off
Hcl reaction, reaction generates the products such as vinylidene chloride, 1,2-dichloroethene, hydrogen chloride.Cracking reaction temperature control is 260
DEG C, air speed is controlled in 10min-1。
Embodiment 5
The spawn obtained by step 1 and 2 is placed in tube furnace, by 20 DEG C of liters with 20 DEG C/min under pure nitrogen gas atmosphere
Warm speed rises to 550 DEG C, and constant temperature 5 hours at this temperature, is cooled to after room temperature and obtains faint yellow product, is ground to powder
After be scattered in HF solution, stir 10 hours, then respectively washing 3 times of deionized water and dehydrated alcohol, 2 are then dried at 50 DEG C
Hour, obtain C3N4Carbon-nitrogen material catalyst.
Obtained catalyst is placed in tube cracking furnace, vinyl trichloride carries out gas phase under catalyst action and takes off
Hcl reaction, reaction generates the products such as vinylidene chloride, 1,2-dichloroethene, hydrogen chloride.Cracking reaction temperature control is 260
DEG C, air speed is controlled in 10min-1。
Table 2 affects for the catalyst prepared under different heating rates on the selectivity of vinylidene chloride, Jing catalysts
After reaction in product inclined two vinyl chloride content, so as to calculate the conversion ratio and selectivity of inclined two vinyl chloride.
Table 2
Embodiment 6
The spawn obtained by step 1 and 2 is placed in tube furnace, under the atmosphere of nitrogen and oxygen by 20 DEG C with 10 DEG C/
The heating rate of min rises to 550 DEG C, and wherein the volume ratio of oxygen and nitrogen is 0.5%, and constant temperature 5 hours at this temperature, cold
But faint yellow product is obtained to room temperature, is ground to after powder and is scattered in HF solution, stirred 10 hours, then deionized water
Respectively wash 3 times with dehydrated alcohol, be then dried 2 hours at 50 DEG C, obtain C3N4Carbon-nitrogen material catalyst.
Obtained catalyst is placed in tube cracking furnace, vinyl trichloride carries out gas phase under catalyst action and takes off
Hcl reaction, reaction generates the products such as vinylidene chloride, 1,2-dichloroethene, hydrogen chloride.Cracking reaction temperature control is 260
DEG C, air speed is controlled in 10min-1。
Embodiment 7
The spawn obtained by step 1 and 2 is placed in tube furnace, under the atmosphere of nitrogen and oxygen by 20 DEG C with 10 DEG C/
The heating rate of min rises to 550 DEG C, and wherein the volume ratio of oxygen and nitrogen is 1.0%, and constant temperature 5 hours at this temperature, cold
But faint yellow product is obtained to room temperature, is ground to after powder and is scattered in HF solution, stirred 10 hours, then deionized water
Respectively wash 3 times with dehydrated alcohol, be then dried 2 hours at 50 DEG C, obtain C3N4Carbon-nitrogen material catalyst.
Obtained catalyst is placed in tube cracking furnace, vinyl trichloride carries out gas phase under catalyst action and takes off
Hcl reaction, reaction generates the products such as vinylidene chloride, 1,2-dichloroethene, hydrogen chloride.Cracking reaction temperature control is 260
DEG C, air speed is controlled in 10min-1。
Embodiment 8
The spawn obtained by step 1 and 2 is placed in tube furnace, under the atmosphere of nitrogen and oxygen by 20 DEG C with 10 DEG C/
The heating rate of min rises to 550 DEG C, and wherein the volume ratio of oxygen and nitrogen is 2.0%, and constant temperature 5 hours at this temperature, cold
But faint yellow product is obtained to room temperature, is ground to after powder and is scattered in HF solution, stirred 10 hours, then deionized water
Respectively wash 3 times with dehydrated alcohol, be then dried 2 hours at 50 DEG C, obtain C3N4Carbon-nitrogen material catalyst.
Obtained catalyst is placed in tube cracking furnace, vinyl trichloride carries out gas phase under catalyst action and takes off
Hcl reaction, reaction generates the products such as vinylidene chloride, 1,2-dichloroethene, hydrogen chloride.Cracking reaction temperature control is 260
DEG C, air speed is controlled in 10min-1。
Embodiment 9
The spawn obtained by step 1 and 2 is placed in tube furnace, under the atmosphere of nitrogen and oxygen by 20 DEG C with 10 DEG C/
The heating rate of min rises to 550 DEG C, and wherein the volume ratio of oxygen and nitrogen is 5.0%, and constant temperature 5 hours at this temperature, cold
But faint yellow product is obtained to room temperature, is ground to after powder and is scattered in HF solution, stirred 10 hours, then deionized water
Respectively wash 3 times with dehydrated alcohol, be then dried 2 hours at 50 DEG C, obtain C3N4Carbon-nitrogen material catalyst.
Obtained catalyst is placed in tube cracking furnace, vinyl trichloride carries out gas phase under catalyst action and takes off
Hcl reaction, reaction generates the products such as vinylidene chloride, 1,2-dichloroethene, hydrogen chloride.Cracking reaction temperature control is 260
DEG C, air speed is controlled in 10min-1。
Table 3 affects for the catalyst prepared under different oxygen content on the selectivity of vinylidene chloride, and Jing catalysts are anti-
The content of inclined two vinyl chloride in rear product is answered, so as to calculate the conversion ratio and selectivity of inclined two vinyl chloride.
Table 3
| Oxygen content/% | Conversion ratio/% | Selectivity/% |
| 0 | 42.83 | 87.55 |
| 0.5 | 52.36 | 90.43 |
| 1.0 | 71.22 | 93.67 |
| 2.0 | 51.89 | 89.82 |
| 5.0 | 39.45 | 67.54 |
The above, is only presently preferred embodiments of the present invention, is not used in the restriction present invention, and those skilled in the art can be
In the essence and protection domain of the present invention, various modifications or equivalent, this modification or equivalent are made to the present invention
Should be regarded as in the protection domain of technical solution of the present invention.
Claims (8)
1. a kind of method of the catalyst for preparing vinylidene chloride by gas-phase catalytic cracking, it is characterised in that：Including following step
Suddenly：
Step 1：A certain amount of dicyanodiamine white powder is added in a certain proportion of pure water, magnetic force is stirred in water bath with thermostatic control
Mix, be completely dissolved dicyanodiamine；
Step 2：A certain proportion of liquid nano silicon dioxide is added in the solution that step 1 is obtained, obtain dicyanodiamine with
The white gels of silicon dioxide；
Step 3：During the white gels material that step 2 is obtained is as tube furnace, in a nitrogen atmosphere by 20 DEG C with certain liter
Warm speed rises to uniform temperature, and keeps temperature constant state at this temperature, is cooled to after room temperature and obtains faint yellow product；
Step 4：The faint yellow product grinding that step 3 is obtained, and be stirred after being scattered in HF solution, then deionized water
Washed and drying with dehydrated alcohol, obtained C3N4Carbon-nitrogen material catalyst；
Step 5：By C3N4Carbon-nitrogen material catalyst is placed in tube cracking furnace, and vinyl trichloride is in C3N4Carbon-nitrogen material is catalyzed
Gas phase dehydrochlorination reaction is carried out under agent effect, reaction generates vinylidene chloride.
2. the method for a kind of catalyst for preparing vinylidene chloride by gas-phase catalytic cracking according to claim 1, its
It is characterised by：The temperature of the constant temperature water bath in the step 1 is 40-60 DEG C, a length of 15min during magnetic agitation.
3. the method for a kind of catalyst for preparing vinylidene chloride by gas-phase catalytic cracking according to claim 1, its
It is characterised by：Heating rate in the step 3 is 5-20 DEG C/min.
4. the method for a kind of catalyst for preparing vinylidene chloride by gas-phase catalytic cracking according to claim 1, its
It is characterised by：The temperature for rising in the step 3 is 400-600 DEG C.
5. the method for a kind of catalyst for preparing vinylidene chloride by gas-phase catalytic cracking according to claim 1, its
It is characterised by：Volume ratio of the nitrogen atmosphere in the step 3 comprising a certain amount of oxygen, oxygen and nitrogen is controlled in 0%-5%.
6. the method for a kind of catalyst for preparing vinylidene chloride by gas-phase catalytic cracking according to claim 1, its
It is characterised by：Deionized water and dehydrated alcohol in the step 4 is respectively washed 2-3 time, and is dried 2 hours at 50 DEG C.
7. the method for a kind of catalyst for preparing vinylidene chloride by gas-phase catalytic cracking according to claim 1, its
It is characterised by：At 260 DEG C, air speed is controlled in 10min the cracking reaction temperature control of the tube cracking furnace in the step 5-1。
8. the method for a kind of catalyst for preparing vinylidene chloride by gas-phase catalytic cracking according to claim 1, its
It is characterised by：The liquid nano silicon dioxide is controlled in 5-10 with the mass ratio of dicyanodiamine.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107216234A (en) * | 2017-06-09 | 2017-09-29 | 浙江三美化工股份有限公司 | A kind of method that use vinylidene chloride catalytic fluorination prepares a fluorine dichloroethanes |
| WO2020220312A1 (en) * | 2019-04-30 | 2020-11-05 | 中国科学院大连化学物理研究所 | Catalyst for preparing vinyl chloride by cracking 1,2-dichloroethane and preparation and regeneration methods therefor |
| CN114471653A (en) * | 2021-12-31 | 2022-05-13 | 山东华夏神舟新材料有限公司 | Catalyst for preparing 1, 1-difluoroethylene by catalytic cracking of chlorodifluoroethane and preparation method and application thereof |
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| CN105417508A (en) * | 2015-12-29 | 2016-03-23 | 哈尔滨工业大学 | Preparation method of macroporous g-C3N4 |
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| JPS5594325A (en) * | 1979-01-11 | 1980-07-17 | Toagosei Chem Ind Co Ltd | Preparation of vinylidene chloride |
| CN105417508A (en) * | 2015-12-29 | 2016-03-23 | 哈尔滨工业大学 | Preparation method of macroporous g-C3N4 |
Non-Patent Citations (1)
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107216234A (en) * | 2017-06-09 | 2017-09-29 | 浙江三美化工股份有限公司 | A kind of method that use vinylidene chloride catalytic fluorination prepares a fluorine dichloroethanes |
| CN107216234B (en) * | 2017-06-09 | 2020-12-08 | 浙江三美化工股份有限公司 | Method for preparing monofluorodichloroethane by catalytic fluorination of vinylidene chloride |
| WO2020220312A1 (en) * | 2019-04-30 | 2020-11-05 | 中国科学院大连化学物理研究所 | Catalyst for preparing vinyl chloride by cracking 1,2-dichloroethane and preparation and regeneration methods therefor |
| US11338276B2 (en) | 2019-04-30 | 2022-05-24 | Dalian Institute Of Chemical Physics, Chinese Academy Of Sciences | Catalyst for preparing chloroethylene by cracking 1,2-dichloroethane and a preparation and regeneration method thereof |
| CN114471653A (en) * | 2021-12-31 | 2022-05-13 | 山东华夏神舟新材料有限公司 | Catalyst for preparing 1, 1-difluoroethylene by catalytic cracking of chlorodifluoroethane and preparation method and application thereof |
| CN114471653B (en) * | 2021-12-31 | 2024-03-26 | 山东华夏神舟新材料有限公司 | Catalyst for preparing 1, 1-difluoroethylene by catalytic pyrolysis of chlorodifluoroethane and preparation method and application thereof |
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Application publication date: 20170517 |