CN105126881A - Method for preparing mercuric chloride catalyst - Google Patents
Method for preparing mercuric chloride catalyst Download PDFInfo
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- CN105126881A CN105126881A CN201510510166.2A CN201510510166A CN105126881A CN 105126881 A CN105126881 A CN 105126881A CN 201510510166 A CN201510510166 A CN 201510510166A CN 105126881 A CN105126881 A CN 105126881A
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Abstract
A disclosed method for preparing a mercuric chloride catalyst is composed of the following processes: (1) performing purifying, screening and drying dewatering on active carbon; (2) putting the active carbon processed in the step (1) and mercuric chloride according to the mass ratio of 7-8:1 into a sealed adsorption tank, controlling the temperature to be 250 DEG C-280 DEG C, the pressure to be 0.1-0.5 MPa and the stirring speed to be 3-4 rpm, so as to enable mercuric chloride to be adsorbed by active carbon in the sealed adsorption tank via a gas-solid phase mass transfer process; keeping a constant temperature, and naturally cooling to room temperature, so as to obtain the mercuric chloride catalyst, and then performing screening to obtain a qualified product; and (3) packaging the qualified product. The effects comprise: a, the technological flow is short, energy consumption is low and product cost is low; b, the method does not generate mercury-containing wastewater or waste gas, and damage to operation workers and environment pollution are reduced; and c, the product quality is high, mercuric chloride in active carbon is uniformly distributed, adsorption is firm, the conversion rate is stable, and the catalyst is long in service life.
Description
Technical field
The present invention relates to the production method in a kind of preparation method of catalyst, be specifically related to a kind of method of the mercuric chleride catalyst for the preparation of polyvinyl chloride.
Background technology
In prior art, be adopt Conventional processing methods preparation with the mercuric chleride catalyst that acetylene synthesizing polyvinyl chloride is used; Namely adopt infusion process, this method is that mercury chloride is mixed with certain density solution, by flooding with active carbon, mercury chloride is made to be adsorbed in active carbon, then by the wet type mercury chloride activated-carbon catalyst of moisture 30%, with heated-air drying 13 hours at 120 DEG C of-130 DEG C of temperature, it is made to be less than 0.3% to moisture, the shortcoming of this infusion process method is that flow process is complicated, production efficiency is low, and energy consumption is high, and three-protection design amount is large, owing to there being certain mercury chloride loss, therefore production cost is also high.
Summary of the invention
The object of the invention is the shortcoming and defect in order to overcome above-mentioned technology, and provide a kind of technological process short, efficiency is high, the production method of the gas phase adsorption method of three-waste free discharge, this method preparing mercuric chleride catalyst avoids the traditional handicraft problem that energy ezpenditure is large in low temperature drying process, also do not have the mercury chloride gas of discharge, contaminated environment, the mercuric chleride catalyst product prepared by the production method of this process can reach GGQ/J7-technical standard.
The present invention prepares the method for mercuric chleride catalyst, adopt mercury chloride distillation time and carrier active carbon directly adsorb in bubble-tight space, therefore this method is also referred to as gas phase adsorption method.
The present invention prepares the method for mercuric chleride catalyst, is adsorbed especially by mercury chloride and carrier active carbon, it is characterized in that it is made up of following procedures with the direct adsorptive gaseous mercury chloride of carrier:
1. active carbon purifying, screening and drying and dehydrating: the purification of carrier active carbon, the screening defective granularity of removing and dirt powder drying and dehydrating, makes it moisturely be less than 0.2%; Again with anhydrous calcium chloride or quick lime dehydrating agent by calcium chloride chemical seasoning process, make its water content be less than 0.1%;
2. adsorption process operation: by the above-mentioned active carbon 1. handled well and mercury chloride in mass ratio for the quality of 7-8:1 puts into the adsorption tanks of sealing, control temperature 250 DEG C-280 DEG C, pressure 0.1-0.5MPa, mixing speed 3-4rpm, the mercury chloride in the adsorption tanks of sealing is made to be sublimed into gaseous state, adsorb mass transport process by vapor solid, and mercury chloride is adsorbed on the activated carbon; After adsorbing chlorinated mercury, absorbent charcoal carrier constant temperature 4 hours at 250 DEG C of-280 DEG C of temperature, naturally cools to room temperature, obtains mercuric chleride catalyst, then obtains qualified products after screening;
3. qualified products packaging: obtain mercuric chleride catalyst qualified products after screening, be packaged to be finished product.
The process units of the preparation method of mercuric chleride catalyst of the present invention is special purpose device, can pass through production requirement self design; It is by active carbon classifying screen 1, whizzer 2, adsorption tanks 3, product sieve 4, qualified catalyst packing machine 5, qualified active carbon 6, drying and dehydrating agent 7, tube rotaring motor 8, thermostat galvanothermy element 9, catalyst prod 10, and active carbon heated drying air heater 11 forms; Due to the process for solid material, formed after a upper operation completes, carry out the Batch Process line apparatus of subsequent processing again, wherein 1. active carbon purifying, screening and drying and dehydrating operation: obtain qualified active carbon 6 from active carbon classifying screen 1, load and whizzer 2, drying and dehydrating agent 7, active carbon heated drying air heater 11 three are linked together in composition drying and dehydrating device, wherein connect with heated dry air pipeline current, carry out drying and dehydrating; 2. adsorption process is born by the adsorption tanks 3 sealed, and it is ensured the process conditions needed in its production method by tube rotaring motor 8, thermostat galvanothermy element 9; 3. the active carbon after adsorbing HgCL2 becomes qualified products and will sieve 4 through product, catalyst prod 10, and qualified catalyst packing machine 5 forms qualified products packaging process successively, and above three process device are arranged in product line device.
The present invention prepares the process units of the method for mercuric chleride catalyst, and active carbon classifying screen 1 sieves reject powder, and removing bulk and impurity, only require granularity 6.5-8.5mm part; The dehydrating agent that drying sloughs moisture content in hot-air used is dry calcium chloride and quick lime; Adsorption tanks are made up of stainless steel or titanium steel material, and tank skin interlayer is equipped with heating and temperature regulating device, can by scope in tank the heating of room temperature 100 DEG C of-400 DEG C of range materials or insulation by, adsorption tanks connect tube rotaring motor 8 and ensure to stir the speed required; Qualified products packing machine 5 is use to obtain mercuric chleride catalyst product 10 and pack after screening removing powder.
The properties of product of the mercuric chleride catalyst prepared by this technique:
Hg chloride content %4.5-6.5
Water content %<0.3
Mechanical strength %>95
Loading density %>550
Li Du ㎜ >6.5
Reach GGQ/J7-technical standard completely.
The carrier active carbon that the present invention is used, in the ordinary course of things, have stronger water absorbing properties, common water absorption rate reaches 70%-80%, for ensureing product quality, in drying and dehydrating process, strictly must control the pressure of container, water price is larger, pressure is larger, and active carbon moisture content is lower, and product quality is higher.
Dried active carbon has again stronger adsorption capacity, and adsorption capacity is not identical at different temperature; And reduce along with the rising of temperature.That is at a certain temperature, can to adsorb and can desorb, sorption and desorption is among dynamic equilibrium all the time, and therefore, in gas-solid phase reaction process, strict temperature control pressure and mixing speed are to ensure the effect of reacting and product quality.
Preparation method of the present invention compares with prior art following effect: a technological process is short, and energy consumption is low, and more capable of reducing energy consumption than general traditional preparation methods 70%, therefore product cost is low; B. mercury-containing waste water, waste gas is not produced, thus the harm reduced operator and environmental pollution; C. product quality is high, and in active carbon, mercury chloride is evenly distributed, and adsorbs firm good catalyst activity, and conversion ratio is stablized, and catalyst life is long.
Accompanying drawing explanation
Fig. 1 technological process of production of the present invention and production equipment schematic diagram.
In FIG, 1. active carbon classifying screen, 2. whizzer, 3. adsorption tanks, 4. product sieve, 5. qualified catalyst packing machine, 6. qualified active carbon, 7. drying and dehydrating agent, 8. tube rotaring motor, 9. thermostat galvanothermy element, 10. catalyst prod.11. active carbon heated drying air heater.
Detailed description of the invention
Below in conjunction with Figure of description, the present invention is described:
The present invention prepares the process units of the method for mercuric chleride catalyst, is special purpose device, can pass through production requirement self design; It is by active carbon classifying screen (1), whizzer (2), adsorption tanks (3), product sieve (4), qualified catalyst packing machine (5), qualified active carbon (6), drying and dehydrating agent (7), tube rotaring motor (8), thermostat galvanothermy element (9), catalyst prod (10), active carbon heated drying air heater (11) forms; Due to the process for solid material, formed after a upper operation completes, carry out the Batch Process line apparatus of subsequent processing again, wherein 1. active carbon purifying, screening and drying and dehydrating operation: obtain qualified active carbon (6) from active carbon classifying screen (1), load and whizzer (2), drying and dehydrating agent (7), active carbon heated drying air heater (11) three are linked together in composition drying and dehydrating device, wherein connect to lead to heated dry air pipeline and carry out drying and dehydrating; 2. adsorption process is born by the adsorption tanks 3 sealed, and it is ensured the process conditions needed in its production method by tube rotaring motor (8), thermostat galvanothermy element (9); 3. the active carbon after adsorbing HgCL2 becomes qualified products and will sieve (4) through product, and catalyst prod (10), qualified catalyst packing machine (5) forms qualified products packaging process successively, and above three process device are arranged in product line device.
The present invention prepares the process units of the method for mercuric chleride catalyst, and active carbon classifying screen 1 sieves reject powder, and removing bulk and impurity, only require granularity 6.5-8.5mm part; The dehydrating agent that drying sloughs moisture content in hot-air used is dry calcium chloride and quick lime; Adsorption tanks are made up of stainless steel or titanium steel material, and tank skin interlayer is equipped with heating and temperature regulating device, can by scope in tank in room temperature 100 DEG C of-400 DEG C of range materials heating or insulation, and adsorption tanks connect tube rotaring motor 8 and ensure to stir the speed required; Qualified products packing machine 5 is use to obtain mercuric chleride catalyst product 10 and pack after screening removing powder.
embodiment 1
Getting granularity is the qualified active carbon of 6.5 ㎜ 350 grams, below drying and dehydrating to 0.2%, takes 50 grams, the dried mercury chloride of anhydrous calcium chloride and makes water content below 0.1%, loads in rotating cylinder synthesizer by above-mentioned active carbon and calcium chloride, closes sealing synthesizer; Synthesize, synthesizer is controlled to heat up, is warmed up to 250 DEG C half an hour, control under 250 DEG C of-260 DEG C of temperature, pressure 0.1-0.2MPa, mixing speed 3-4rpm, make mercury chloride be sublimed into gaseous state, be tightly held by activated carbon, at 250 DEG C of-260 DEG C of temperature, constant temperature is after 4 hours again, naturally cool to room temperature, obtain mercuric chleride catalyst, then through screening, discard the product being less than 6.5 ㎜, obtain qualified products.
embodiment 2
Getting granularity is the qualified active carbon of 6.5 ㎜ 500 grams, below drying and dehydrating to 0.2%, takes 65 grams, the dried mercury chloride of anhydrous calcium chloride, makes water content below 0.1%, loads in rotating cylinder synthesizer by above-mentioned active carbon and calcium chloride, closes sealing synthesizer; Synthesize, synthesizer is controlled to heat up, is warmed up to 260 DEG C half an hour, control at 260 DEG C of-270 DEG C of temperature, pressure 0.2-0.3MPa, mixing speed 3-4rpm, make mercury oxide be sublimed into gaseous state, be tightly held by activated carbon, at 260 DEG C of-270 DEG C of temperature, constant temperature is after 4 hours, naturally cool to room temperature, obtain mercuric chleride catalyst, then through screening, abandon the product being less than 6.5 ㎜, obtain qualified products.
embodiment 3
Getting granularity is the qualified active carbon of 6.5 ㎜ 1000 grams, below drying and dehydrating to 0.2%, takes 130 grams, the dried mercury chloride of anhydrous calcium chloride, makes water content below 0.1%, loads in rotating cylinder synthesizer by above-mentioned active carbon and calcium chloride, closes sealing synthesizer; Synthesize, synthesizer is controlled to heat up, is warmed up to 270 DEG C half an hour, control at 270 DEG C of-280 DEG C of temperature, pressure 0.3-0.5MPa, mixing speed 3-4rpm, then at 270 DEG C of-280 DEG C of temperature, constant temperature is after 4 hours, naturally cool to room temperature, obtain mercuric chleride catalyst, abandon the product being less than 6.5 ㎜, again through screening, obtain qualified products.
Claims (3)
1. prepare a method for mercuric chleride catalyst, it is characterized in that it is made up of following procedures with the direct adsorptive gaseous mercury chloride of carrier:
1. active carbon purifying, screening and drying and dehydrating: the purification of carrier active carbon, the screening defective granularity of removing and dirt powder drying and dehydrating, makes it moisturely be less than 0.2%; Again with anhydrous calcium chloride or quick lime dehydrating agent by calcium chloride chemical seasoning process, make its water content be less than 0.1%;
2. adsorption process: by the above-mentioned active carbon 1. handled well and mercury chloride in mass ratio for the quality of 7-8:1 puts into the adsorption tanks of sealing, control temperature 250 DEG C-280 DEG C, pressure 0.1-0.5MPa, mixing speed 3-4rpm, the mercury chloride in the adsorption tanks of sealing is made to be sublimed into gaseous state, adsorb mass transport process by vapor solid, and mercury chloride is adsorbed on the activated carbon; After adsorbing chlorinated mercury, absorbent charcoal carrier constant temperature 4 hours at 250 DEG C of-280 DEG C of temperature, naturally cools to room temperature, obtains mercuric chleride catalyst, then obtains qualified products after screening;
3. qualified products packaging: obtain mercuric chleride catalyst qualified products after screening, be packaged to be finished product.
2. prepare the process units of the method for mercuric chleride catalyst for one kind, it is characterized in that by active carbon classifying screen (1), whizzer (2), adsorption tanks (3), product sieve (4), qualified catalyst packing machine (5), qualified active carbon (6), drying and dehydrating agent (7), tube rotaring motor (8), thermostat galvanothermy element (9), catalyst prod (10), active carbon heated drying air heater (11) forms; Because material is solid matter, production process by product: 1. active carbon purifying, screening and drying and dehydrating: 2. adsorption process: in the adsorption tanks of sealing, 3. qualified products are packed three process device and are arranged in product line device, formed after a upper operation completes, then carry out the Batch Process line apparatus of subsequent processing.
3. prepare a process units for the method for mercuric chleride catalyst, it is characterized in that the purifier of carrier active carbon, active carbon classifying screen (1) sieve reject powder, removing bulk and impurity, only require granularity 6.5-8.5mm part; The dehydrating agent device that drying sloughs moisture content in hot-air used is dry calcium chloride and quick lime; Adsorption tanks (3) are made up of stainless steel or titanium steel material, tank skin interlayer is equipped with heating (9) and temperature regulating device, can by scope in tank in room temperature 100 DEG C of-400 DEG C of range materials heating or insulation, adsorption tanks (3) connect tube rotaring motor (8) and ensure to stir the speed required; Qualified products packing machine (5) is use to obtain mercuric chleride catalyst product (10) and pack after screening removing powder.
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1067594A (en) * | 1991-06-11 | 1993-01-06 | 贵州汞矿 | Method for preparing mercuric chloride catalyst |
CN102764560A (en) * | 2012-08-02 | 2012-11-07 | 长葛市九州化工有限公司 | Method for purifying waste gas in mercury catalyst production |
CN202555136U (en) * | 2012-05-05 | 2012-11-28 | 长葛市九州化工有限公司 | Tail gas purification device for mercuric chloride catalyst production |
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- 2015-08-19 CN CN201510510166.2A patent/CN105126881A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1067594A (en) * | 1991-06-11 | 1993-01-06 | 贵州汞矿 | Method for preparing mercuric chloride catalyst |
CN202555136U (en) * | 2012-05-05 | 2012-11-28 | 长葛市九州化工有限公司 | Tail gas purification device for mercuric chloride catalyst production |
CN102764560A (en) * | 2012-08-02 | 2012-11-07 | 长葛市九州化工有限公司 | Method for purifying waste gas in mercury catalyst production |
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Application publication date: 20151209 |