CN107715902A - A kind of gas-solid phase chloromethanes catalyst and its preparation method - Google Patents
A kind of gas-solid phase chloromethanes catalyst and its preparation method Download PDFInfo
- Publication number
- CN107715902A CN107715902A CN201710790824.7A CN201710790824A CN107715902A CN 107715902 A CN107715902 A CN 107715902A CN 201710790824 A CN201710790824 A CN 201710790824A CN 107715902 A CN107715902 A CN 107715902A
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- China
- Prior art keywords
- catalyst
- gas
- solid phase
- chloromethanes
- preparation
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/138—Halogens; Compounds thereof with alkaline earth metals, magnesium, beryllium, zinc, cadmium or mercury
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/04—Mixing
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/088—Decomposition of a metal salt
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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
- C07C17/16—Preparation of halogenated hydrocarbons by replacement by halogens of hydroxyl groups
Abstract
The invention discloses a kind of gas-solid phase chloromethanes catalyst and its preparation method, a kind of gas-solid phase chloromethanes catalyst, consist of the following composition, high-purity alpha-alumina, activated carbon, methanol, ammonium chloride, hydrogen chloride, zinc chloride, calcium hydroxide and sodium hydroxide, a kind of preparation method of gas-solid phase chloromethanes catalyst, including 5 steps, respectively make carrier, make active material, blending, mediate and be granulated and dry roast, the selectivity of chloromethanes is effectively increased by catalyst made from a kind of gas-solid phase chloromethanes catalyst of the present invention and its preparation method, environment-friendly high-efficiency, efficiency high can be recycled, service life is grown, it is generally applicable in Catalyst Production industry.
Description
Technical field
The present invention relates to the production method of industrial chemicals, is to be related to a kind of gas-solid phase chloromethanes catalysis more particularly
Agent and its preparation method.
Background technology
In recent years, China's methanol hydrogen chloride technology obtained very big development, and hydrogen chloride technology mainly has liquid catalytic
With two kinds of gas-phase catalysis, because gas-phase catalysis production process is simple, easily controllable and large-scale production, so a wide range of
Use, however, the catalyst effect in gas and solid phase catalytic is more preferably.
The content of the invention
Goal of the invention：The purpose of the present invention is to be directed to prior art deficiency and defect, there is provided a kind of gas-solid phase chloromethanes is urged
Agent and its preparation method, there is good catalytic effect according to catalyst made of technical scheme provided by the present invention.
Technical scheme：To achieve these goals, the technical solution adopted in the present invention is：A kind of gas-solid phase chloromethanes is urged
Agent and its preparation method.
A kind of gas-solid phase chloromethanes catalyst, is consisted of the following composition, high-purity alpha-alumina, activated carbon, methanol, chlorination
Ammonium, hydrogen chloride, zinc chloride, calcium hydroxide and sodium hydroxide, each constituent press mass fraction percentage：
The material of replacing of the activated carbon is one or more of combinations in diatomite, molecular sieve, kaolin and silica gel
Thing.
A kind of preparation method of gas-solid phase chloromethanes catalyst：
Step A：Make carrier first, activated carbon is put into grinder, after activated carbon is ground into required fineness, then will grind
The activated carbon of milled is put into agitator, and slowly the 1/3 of multiple addition methanol total amount, stirs 5min, take out, be placed on clean
It is stand-by in container；
Step B：Active material is made by high-purity alpha-alumina, ammonium chloride, hydrogen chloride, zinc chloride, calcium hydroxide and hydrogen-oxygen
Change sodium, which is placed in another clean agitator, to stir, when high-purity alpha-alumina, ammonium chloride, hydrogen chloride, zinc chloride, hydrogen
Calcium oxide and sodium hydroxide, the 1/3 of methanol total amount is added while stirring, after required methanol adds, continue to stir 10min, take
Go out, be placed in another clean container, it is stand-by；
Step C：Active material in carrier in step A and step B is added separately to a clean stirring by blending
In bucket, the 1/6 of methanol the residuals on the container inner wall in step A and step B are rinsed respectively needed for this step institute
In agitator, stirring 10min obtains blend；
Step D：Mediate to be granulated and add the blend in step C to comminutor, obtain mixture, coarse grained mix is entered
Row screening, meet that the particulate mixtures of fineness requirement enter and handle in next step, the particulate mixtures for being unsatisfactory for fineness requirement crush
Afterwards, return to step C is re-worked；
Step E：Dry roast and the particulate mixtures obtained in step C are put into baking oven 3min, after drying, roast 15min.
The mixing speed of mixer is 1500rad/min in step A and step B, the stirring speed of mixer in the step C
Spend for 2500rad/min.
It is 250-350 mesh that fineness is sieved in the step C.
Beneficial effect：Compared with prior art, its advantage is the present invention：
Chloromethanes is effectively increased by catalyst made from a kind of gas-solid phase chloromethanes catalyst of the present invention and its preparation method
Selectivity, environment-friendly high-efficiency can be recycled efficiency high, and service life length is generally applicable in Catalyst Production industry.
Embodiment
With reference to embodiment, the present invention is further illustrated.
A kind of gas-solid phase chloromethanes catalyst, is consisted of the following composition, high-purity alpha-alumina, activated carbon, methanol, chlorination
Ammonium, hydrogen chloride, zinc chloride, calcium hydroxide and sodium hydroxide, each constituent is according to composition required for making 100g catalyst
Quality meter：
A kind of preparation method of gas-solid phase chloromethanes catalyst：
Step A：Make carrier first, activated carbon is put into grinder, after activated carbon is ground into required fineness, then will grind
The activated carbon of milled is put into agitator, slowly multiple addition methanol 3g, stirs 5min, takes out, is placed in clean container,
It is stand-by；
Step B：Active material is made by high-purity alpha-alumina, ammonium chloride, hydrogen chloride, zinc chloride, calcium hydroxide and hydrogen-oxygen
Change sodium, which is placed in another clean agitator, to stir, when high-purity alpha-alumina, ammonium chloride, hydrogen chloride, zinc chloride, hydrogen
After calcium oxide and sodium hydroxide stir, methanol 3g is added while stirring, after required methanol adds, continues to stir 10min,
Take out, be placed in another clean container, it is stand-by；
Step C：Active material in carrier in step A and step B is added separately to a clean stirring by blending
In bucket, methanol 1.5g rinses the residuals on the container inner wall in step A and step B to used in this step needed for respectively
Agitator in, stirring 10min obtain blend；
Step D：Mediate to be granulated and add the blend in step C to comminutor, obtain mixture, coarse grained mix is entered
Row screening, meet that the particulate mixtures of fineness requirement enter and handle in next step, the particulate mixtures for being unsatisfactory for fineness requirement crush
Afterwards, return to step C is re-worked；
Step E：Dry roast and the particulate mixtures obtained in step C are put into baking oven 3min, after drying, roast 15min.
It is complete by above-mentioned description, relevant staff using the above-mentioned desirable embodiment according to the present invention as enlightenment
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The present invention's is technical
Scope is not limited to the content on specification, it is necessary to determines its technical scope according to right.
Claims (5)
- A kind of 1. gas-solid phase chloromethanes catalyst, it is characterised in that：Consist of the following composition, high-purity alpha-alumina, activated carbon, first Alcohol, ammonium chloride, hydrogen chloride, zinc chloride, calcium hydroxide and sodium hydroxide, each constituent press mass fraction percentage：
- A kind of 2. gas-solid phase chloromethanes catalyst according to claim 1, it is characterised in that：The alternative of told activated carbon Matter is one or more of compositions in diatomite, molecular sieve, kaolin and silica gel.
- A kind of 3. preparation method of gas-solid phase chloromethanes catalyst, it is characterised in that：Step A：Make carrier first, activated carbon is put into grinder, after activated carbon is ground into required fineness, then will be ground Activated carbon be put into agitator, slowly the 1/3 of multiple addition methanol total amount, stirs 5min, takes out, be placed on clean container In, it is stand-by；Step B：Active material is made by high-purity alpha-alumina, ammonium chloride, hydrogen chloride, zinc chloride, calcium hydroxide and sodium hydroxide It is placed in another clean agitator and stirs, when high-purity alpha-alumina, ammonium chloride, hydrogen chloride, zinc chloride, hydroxide After calcium and sodium hydroxide stir, methanol 3g is added while stirring, after required methanol adds, is continued to stir 10min, is taken Go out, be placed in another clean container, it is stand-by；Step C：Active material in carrier in step A and step B is added separately in a clean agitator by blending, The 1/6 of methanol the residuals on the container inner wall in step A and step B are rinsed respectively needed for stirring used in this step Mix in bucket, stirring 10min obtains blend；Step D：Mediate to be granulated and add the blend in step C to comminutor, obtain mixture, coarse grained mix is sieved Point, meet that the particulate mixtures of fineness requirement enter and handle in next step, after being unsatisfactory for the particulate mixtures crushing of fineness requirement, return Step C is returned to re-work；Step E：Dry roast and the particulate mixtures obtained in step C are put into baking oven 3min, after drying, roast 15min.
- A kind of 4. preparation method of gas-solid phase chloromethanes catalyst according to claim 3, it is characterised in that：Step A and step B The mixing speed of middle mixer is 1500rad/min, and the mixing speed of mixer is 2500rad/min in the step C.
- A kind of 5. preparation method of gas-solid phase chloromethanes catalyst, it is characterised in that：It is 250-350 that fineness is sieved in the step C Mesh.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710790824.7A CN107715902A (en) | 2017-09-05 | 2017-09-05 | A kind of gas-solid phase chloromethanes catalyst and its preparation method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710790824.7A CN107715902A (en) | 2017-09-05 | 2017-09-05 | A kind of gas-solid phase chloromethanes catalyst and its preparation method |
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| CN107715902A true CN107715902A (en) | 2018-02-23 |
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| CN201710790824.7A Pending CN107715902A (en) | 2017-09-05 | 2017-09-05 | A kind of gas-solid phase chloromethanes catalyst and its preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112657486A (en) * | 2020-12-13 | 2021-04-16 | 中海油天津化工研究设计院有限公司 | Preparation method of catalyst for preparing methane chloride from methanol by gas phase method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1347862A (en) * | 2001-10-08 | 2002-05-08 | 浙江衢化氟化学有限公司 | Gas and solid phase catalytic process of synthesizing methane chloride |
-
2017
- 2017-09-05 CN CN201710790824.7A patent/CN107715902A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1347862A (en) * | 2001-10-08 | 2002-05-08 | 浙江衢化氟化学有限公司 | Gas and solid phase catalytic process of synthesizing methane chloride |
| CN1164543C (en) * | 2001-10-08 | 2004-09-01 | 浙江衢化氟化学有限公司 | Gas and solid phase catalytic process of synthesizing methane chloride |
Non-Patent Citations (1)
| Title |
|---|
| 魏士东等: "甲醇氯化铵法合成氯甲烷催化剂", 《化学反应工程与工艺》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112657486A (en) * | 2020-12-13 | 2021-04-16 | 中海油天津化工研究设计院有限公司 | Preparation method of catalyst for preparing methane chloride from methanol by gas phase method |
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