阅读说明：本技术 一种四氯化碳转氯仿催化剂的制备方法 (Preparation method of catalyst for converting carbon tetrachloride into chloroform ) 是由 夏旭东 龚英俊 于 2020-07-23 设计创作，主要内容包括：本发明公开了一种四氯化碳转氯仿催化剂的制备方法,配方包括：氯铂酸、二氯甲烷、氧化铝、氯化钾、乙酸、草酸、去离子水、锰单体和吸附剂,各组分的质量百分含量分别是：15-25%的氯铂酸、20-35%的二氯甲烷、15-25%的氧化铝、10-20%的氯化钾、2-4%的乙酸、10-20%的草酸、1-3%的去离子水、6-11%的锰单体和0.5-1%的吸附剂；该发明,安全可靠,采用氧化铝与氯铂酸作为载体制成四氯化碳转氯仿催化剂,摒弃传统采用催化加氢反应方式,吸附剂剪裁浸渍更有利于载体加工,二氯甲烷作为稀释剂添加,更加增加该四氯化碳转氯仿催化剂催化效率,有利于四氯化碳转氯仿催化,催化剂活性强,转换率高,且该发明工艺简单严谨,原料便宜成本低廉,大大节约了生产成本。(The invention discloses a preparation method of a catalyst for converting carbon tetrachloride into chloroform, which comprises the following steps: chloroplatinic acid, dichloromethane, aluminum oxide, potassium chloride, acetic acid, oxalic acid, deionized water, a manganese monomer and an adsorbent, wherein the mass percentages of the components are as follows: 15-25% of chloroplatinic acid, 20-35% of dichloromethane, 15-25% of alumina, 10-20% of potassium chloride, 2-4% of acetic acid, 10-20% of oxalic acid, 1-3% of deionized water, 6-11% of manganese monomer and 0.5-1% of adsorbent; the method is safe and reliable, the catalyst for converting carbon tetrachloride into chloroform is prepared by adopting alumina and chloroplatinic acid as carriers, the traditional catalytic hydrogenation reaction mode is abandoned, the carrier processing is more favorably realized by cutting and soaking an adsorbent, the dichloromethane is added as a diluent, the catalytic efficiency of the catalyst for converting carbon tetrachloride into chloroform is more increased, the catalyst for converting carbon tetrachloride into chloroform is favorably catalyzed, the activity of the catalyst is strong, the conversion rate is high, the process is simple and precise, the raw materials are cheap, the cost is low, and the production cost is greatly saved.)

1. A catalyst for converting carbon tetrachloride into chloroform is characterized in that: the formula comprises the following components: chloroplatinic acid, dichloromethane, aluminum oxide, potassium chloride, acetic acid, oxalic acid, deionized water, a manganese monomer and an adsorbent, wherein the mass percentages of the components are as follows: 15-25% of chloroplatinic acid, 20-35% of dichloromethane, 15-25% of alumina, 10-20% of potassium chloride, 2-4% of acetic acid, 10-20% of oxalic acid, 1-3% of deionized water, 6-11% of manganese monomer and 0.5-1% of adsorbent.

2. A preparation method of a catalyst for converting carbon tetrachloride into chloroform comprises the following steps of selecting raw materials; step two, cutting and dipping; step three, drying and reducing; step four, catalyst treatment; step five, packaging and storing; the method is characterized in that:

in the first step, the components in percentage by mass are as follows: selecting 15-25% chloroplatinic acid, 20-35% dichloromethane, 15-25% alumina, 10-20% potassium chloride, 2-4% acetic acid, 10-20% oxalic acid, 1-3% deionized water, 6-11% manganese monomer and 0.5-1% adsorbent, and weighing according to the weight percentage sum of 1;

in the second step, the cutting and dipping comprises the following steps:

1) cleaning the adsorbent, manually cutting to a size of 1cm²The ground pieces of (a);

2) cleaning the reaction kettle, adding the cut adsorbent, adding deionized water into the reaction kettle, and continuously stirring for 10-20 min;

3) keeping the temperature of the material, and slowly pouring chloroplatinic acid into the reaction kettle while stirring; stirring for 10-20min, reducing material temperature, maintaining at 10-20 deg.C, and standing for 1-2 hr;

in the third step, the drying and reducing step comprises the following steps:

1) manually filtering the surface water of the mixture obtained in the step two 3), standing for 1-2h, and then putting into a drying oven;

2) adding dichloromethane and alumina, heating to 70-90 deg.C, and reacting for 20-40 min;

3) manually pouring out the mixture after reaction, and naturally cooling the mixture in a cool place to obtain a catalyst precursor M;

in the fourth step, the catalyst treatment comprises the following steps:

1) pouring the mixture obtained in the step three 3) into a centrifuge, adding potassium chloride and oxalic acid, starting the centrifuge for processing for 10-20min, and then pouring into a reaction kettle;

2) adding acetic acid into the reaction kettle, standing for 10-20min, adding a manganese monomer, and reacting for 1-2h to obtain a catalyst precursor M₂；

3) Catalyst precursor M₂Pouring the mixture into a tubular muffle furnace, and introducing hydrogen to carry out reduction reaction to obtain a catalyst for converting carbon tetrachloride into chloroform;

in the fifth step, the carbon tetrachloride-chloroform catalyst obtained in the fourth step 2) is packaged in boxes, the same weight of each box is ensured, and the carbon tetrachloride-chloroform catalyst packaged in boxes is packaged and stored in boxes integrally.

3. A catalyst as claimed in claim 1, wherein: the components are as follows by mass percent: 16% of chloroplatinic acid, 25% of dichloromethane, 20% of aluminum oxide, 10% of potassium chloride, 4% of acetic acid, 10% of oxalic acid, 3% of deionized water, 11% of dichloromethane and 1% of adsorbent.

4. A catalyst as claimed in claim 1, wherein: the adsorbent is activated carbon.

5. The method for preparing a catalyst for converting carbon tetrachloride into chloroform according to claim 2, wherein: the processing temperature in the second step 2) is 40-60 ℃.

6. The method for preparing a catalyst for converting carbon tetrachloride into chloroform according to claim 2, wherein: stirring once every 10min during reaction in the step three 2).

7. The method for preparing a catalyst for converting carbon tetrachloride into chloroform according to claim 2, wherein: the reaction temperature in the step four 2) is 60-80 ℃.

8. The method for preparing a catalyst for converting carbon tetrachloride into chloroform according to claim 2, wherein: and in the fifth step, the catalyst for converting carbon tetrachloride into chloroform needs to be stored in a shady place.

Technical Field

The invention relates to the technical field of carbon tetrachloride-chloroform conversion, in particular to a preparation method of a catalyst for converting carbon tetrachloride into chloroform.

Background

Chloroform, also known as trichloromethane, is a colorless transparent liquid, has special smell, sweet taste, high refraction, non-combustibility, heavy weight, volatility, is photosensitive, can be gradually decomposed under illumination with oxygen in the air to generate virulent phosgene hydrogen chloride, carbon tetrachloride is generally adopted for chloroform conversion reaction, a catalyst is required for catalytic reaction for the conversion of carbon tetrachloride to chloroform, a hydrogenation reaction mode is adopted for the traditional conversion of carbon tetrachloride to chloroform, the catalytic efficiency of the catalyst for the conversion of carbon tetrachloride to chloroform is reduced, the catalysis for the conversion of carbon tetrachloride to chloroform is not facilitated, the catalyst activity is poor, the service life is short, the conversion rate is low, and the traditional conversion of carbon tetrachloride to chloroform catalyst is expensive in raw materials, troublesome to process, the production cost is increased, and the processing and production of the catalyst for the conversion; in view of these drawbacks, it is necessary to design a method for preparing a carbon tetrachloride to chloroform catalyst.

Disclosure of Invention

The invention aims to provide a preparation method of a catalyst for converting carbon tetrachloride into chloroform, which aims to solve the problems in the background technology.

In order to solve the technical problems, the invention provides the following technical scheme: a catalyst for converting carbon tetrachloride into chloroform comprises the following components: chloroplatinic acid, dichloromethane, aluminum oxide, potassium chloride, acetic acid, oxalic acid, deionized water, a manganese monomer and an adsorbent, wherein the mass percentages of the components are as follows: 15-25% of chloroplatinic acid, 20-35% of dichloromethane, 15-25% of alumina, 10-20% of potassium chloride, 2-4% of acetic acid, 10-20% of oxalic acid, 1-3% of deionized water, 6-11% of manganese monomer and 0.5-1% of adsorbent.

A preparation method of a catalyst for converting carbon tetrachloride into chloroform comprises the following steps of selecting raw materials; step two, cutting and dipping; step three, drying and reducing; step four, catalyst treatment; step five, packaging and storing;

in the first step, the components in percentage by mass are as follows: selecting 15-25% chloroplatinic acid, 20-35% dichloromethane, 15-25% alumina, 10-20% potassium chloride, 2-4% acetic acid, 10-20% oxalic acid, 1-3% deionized water, 6-11% manganese monomer and 0.5-1% adsorbent, and weighing according to the weight percentage sum of 1;

in the second step, the cutting and dipping comprises the following steps:

1) cleaning the adsorbent, manually cutting to a size of 1cm²The ground pieces of (a);

2) cleaning the reaction kettle, adding the cut adsorbent, adding deionized water into the reaction kettle, and continuously stirring for 10-20 min;

3) keeping the temperature of the material, and slowly pouring chloroplatinic acid into the reaction kettle while stirring; stirring for 10-20min, reducing material temperature, maintaining at 10-20 deg.C, and standing for 1-2 hr;

in the third step, the drying and reducing step comprises the following steps:

1) manually filtering the surface water of the mixture obtained in the step two 3), standing for 1-2h, and then putting into a drying oven;

2) adding dichloromethane and alumina, heating to 70-90 deg.C, and reacting for 20-40 min;

3) manually pouring out the mixture after reaction, and naturally cooling the mixture in a cool place to obtain a catalyst precursor M;

in the fourth step, the catalyst treatment comprises the following steps:

1) pouring the mixture obtained in the step three 3) into a centrifuge, adding potassium chloride and oxalic acid, starting the centrifuge for processing for 10-20min, and then pouring into a reaction kettle;

2) adding acetic acid into the reaction kettle, standing for 10-20min, adding a manganese monomer, and reacting for 1-2h to obtain a catalyst precursor M₂；

3) Catalyst precursor M₂Pouring the mixture into a tubular muffle furnace, and introducing hydrogen to carry out reduction reaction to obtain a catalyst for converting carbon tetrachloride into chloroform;

in the fifth step, the carbon tetrachloride-chloroform catalyst obtained in the fourth step 2) is packaged in boxes, the same weight of each box is ensured, and the carbon tetrachloride-chloroform catalyst packaged in boxes is packaged and stored in boxes integrally.

According to the technical scheme, the components are as follows by mass percent: 16% of chloroplatinic acid, 25% of dichloromethane, 20% of aluminum oxide, 10% of potassium chloride, 4% of acetic acid, 10% of oxalic acid, 3% of deionized water, 11% of manganese monomer and 1% of adsorbent.

According to the technical scheme, the adsorbent is activated carbon.

According to the technical scheme, the processing temperature in the second step 2) is 40-60 ℃.

According to the technical scheme, the reaction in the step three 2) is stirred once every 10 min.

According to the technical scheme, the reaction temperature in the step four 2) is 60-80 ℃.

According to the technical scheme, in the fifth step, the catalyst for converting carbon tetrachloride into chloroform needs to be stored in a shady place.

Compared with the prior art, the invention has the following beneficial effects: the method is safe and reliable, the catalyst for converting carbon tetrachloride into chloroform is prepared by adopting alumina and chloroplatinic acid as carriers, the traditional catalytic hydrogenation reaction mode is abandoned, the carrier processing is more favorably realized by cutting and soaking an adsorbent, the dichloromethane is added as a diluent, the catalytic efficiency of the catalyst for converting carbon tetrachloride into chloroform is more increased, the catalyst for converting carbon tetrachloride into chloroform is favorably converted, the catalyst is strong in activity, long in service life and high in conversion rate, the method is simple and rigorous in process, can replace other expensive processes for converting carbon tetrachloride into chloroform, the effect is remarkable, the raw materials are cheap, the processing is convenient, the production cost is greatly saved, and the processing production of the catalyst for converting carbon tetrachloride into chloroform is favorably realized.

Drawings

The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:

FIG. 1 is a process flow diagram of the present invention.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Referring to fig. 1, the present invention provides a technical solution: a preparation method of a catalyst for converting carbon tetrachloride into chloroform comprises the following steps: