CN106629604B - A method of gas phase chlorination hydrogen is produced using chlorosilane raffinate - Google Patents
A method of gas phase chlorination hydrogen is produced using chlorosilane raffinate Download PDFInfo
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- CN106629604B CN106629604B CN201611060430.8A CN201611060430A CN106629604B CN 106629604 B CN106629604 B CN 106629604B CN 201611060430 A CN201611060430 A CN 201611060430A CN 106629604 B CN106629604 B CN 106629604B
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- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
The invention discloses a kind of methods for producing gas phase chlorination hydrogen using chlorosilane raffinate, belong to polysilicon raffinate process field；When reaction is hydrolyzed in chlorosilane raffinate, make reaction in high-concentration sulfuric acid atmosphere, sulfuric acid show water imbibition make hydrogen chloride gas in a liquid extremely difficult dissolution and volatilize and gas phase be presented, the chlorosilane raffinate of hydrogen and vaporization that hydrogen chloride gas and hydrolysis generate, which successively enters after condenser, high-pressure separator processing to separate, obtains chlorination hydrogen production.Technological process of production advantages of simple of the present invention is able to solve the resource utilization problem of chlorosilane raffinate, high efficiente callback hydrogen chloride.
Description
Technical field
The invention discloses a kind of methods for taking hydrogen chloride using chlorosilane raffinate gas phase, belong to the processing of polysilicon raffinate
Field.
Background technique
Sulfuric acid is a kind of most active binary inorganic acid, and the sulfuric acid of high concentration has strong water imbibition, in organic synthesis
It can be used as dehydrating agent.
Improved Siemens are Now Domestic production polysilicon prevailing technologies, produce polysilicon process in improved Siemens
Middle trichlorosilane synthesis, the rectification and purification of trichlorosilane, trichlorosilane reduction and cold (heat) hydrogenation process all can have chlorosilane residual
Liquid generates.Main component: polychlorostyrene silane, SiCl4、SiHCl3、SiH2Cl2, HCl, a small amount of silicon powder and metal chloride.At present
The processing of most domestic polysilicon factory chlorosilane raffinate is absorbed into absorption tower by lye after being mixed with raffinate with nitrogen,
Sodium metasilicate and sodium chloride mixed solution are finally obtained, separating difficulty is big, separation purity is low, and product use scope is narrow, causes chlorine silicon
The wasting of resources of alkane raffinate, or even cause the chlorine pollution to environment.
Hydrogen chloride is in modern industrial production using very wide a kind of chemicals, as the regulator of solution acid alkalinity,
The fields such as dyestuff, fragrance, drug are as raw material, the effects of can be carried out organic catalyst compound, solvent, corrosive agent.Modern chlor-alkali
Industry is to the identity output that the production of hydrogen chloride is with byproduct mostly, and impure type is more in byproduct, impurity level is big,
It need to obtain meeting industrial chlorination hydrogen production by a large amount of purification & isolations.
The mainly SiCl of reaction is participated in when chlorosilane raffinate hydrolyzes4、SiHCl3、SiH2Cl2Three kinds of substances, mainly generate
Three kinds of silica, hydrogen chloride gas, hydrogen substances.
Summary of the invention
It is residual in chlorosilane the purpose of the present invention is to provide a kind of method for producing gas phase chlorination hydrogen using chlorosilane raffinate
When reaction is hydrolyzed in liquid, make reaction in high-concentration sulfuric acid atmosphere, sulfuric acid, which shows water imbibition, makes hydrogen chloride gas in liquid
Extremely difficult dissolution in body and volatilize and gas phase be presented, the chlorosilane raffinate of hydrogen chloride and the hydrolysis hydrogen generated and vaporization is successive
It is separated after into condenser, high-pressure separator processing and obtains chlorination hydrogen production；Production procedure advantages of simple of the present invention, can solve
The certainly resource utilization problem of chlorosilane raffinate, high efficiente callback hydrogen chloride；Specifically includes the following steps:
(1) sulfuric acid solution is placed in stirred autoclave 1, then chlorosilane raffinate is slowly dropped in sulfuric acid solution,
Being stirred continuously is uniformly mixed reactant, wherein the mass percent concentration of sulfuric acid solution is more than or equal to 20%；
(2) being continuously added with chlorosilane raffinate, the gas generated in reaction kettle (main component be hydrogen chloride gas,
Hydrogen, gas phase chlorosilane raffinate) enter in condenser 6, the liquid phase substance being condensed out returns in stirred autoclave 1, gaseous substance
Into in high-pressure separator 7, the liquid phase substance isolated is recycled respectively with gaseous substance, liquefied hydrogen chloride is in room temperature
Become the hydrogen chloride of gas phase under normal pressure；
(3) silicon dioxide colloid that hydrolysis generates floats because density is less than sulfuric acid, will be stirred by Pulp pump 2 anti-
It answers the slurry on kettle top to be extracted into filter press 3 and carries out filters pressing, filtrate (sulfuric acid concentration 65%-75%) enters sulfuric acid filtrate accumulator tank 5
The concentration (sulfuric acid concentration maintains between 20%-60%) of middle industry moisturizing adjustment sulfuric acid filtrate returns to stirring after pumping 4 by peracid
In reaction kettle 1.
Preferably, the temperature of condenser 6 of the present invention is -30 ~ -15 DEG C, and the liquefaction of gas phase chlorosilane raffinate is made to return to water
Solution, hydrogen chloride gas and two kinds of substances of hydrogen enter high-pressure separator 7 with gas phase state, and the pressure of control high-pressure separator 7 is
Between 1.9 ~ 2.5Mpa, hydrogen chloride gas liquefaction and Hydrogen Separation come, and the hydrogen chloride purity of gas phase is up to 94%-97%, recycling
Rate is greater than 85%, and energy recycle is in polycrystalline silicon production system and using in more chlor-alkali compound probability.
Preferably, chlorosilane raffinate hydrolysis temperature controls between 20 DEG C -50 DEG C in stirred autoclave 1 of the present invention.
Preferably, the mass percent concentration of sulfuric acid solution described in step (1) of the present invention is 20%-60%, and chlorosilane is residual
The charge-mass ratio of liquid and sulfuric acid solution is 11:50-16:5.
Another object of the present invention is to provide a kind of devices that gas phase chlorination hydrogen is produced using chlorosilane raffinate, including stir
Reaction kettle 1, Pulp pump 2, filter press 3, acid pump 4, sulfuric acid filtrate accumulator tank 5, condenser 6, high-pressure separator 7 are mixed, are stirred to react
The upper end of kettle 1 is connected to chlorosilane raffinate storage device, and lower end is connected to by Pulp pump 2 with filter press 3, filter press 3 and sulfuric acid
Filtrate accumulator tank 5 is connected to, and the lower end of sulfuric acid filtrate accumulator tank 5 is connected to by acid pump 4 with stirred autoclave 1；The recycling of sulfuric acid filtrate
Slot 5, stirred autoclave 1 upper end be connected to condenser 6, the lower end of condenser 6 is connected to stirred autoclave 1, condenser 6 with
High-pressure separator 7 is connected to.
The principle of the present invention:
Chlorosilane raffinate will generate hydrogen chloride gas when hydrolyzing, and the present invention mainly utilizes chlorosilane raffinate, the concentrated sulfuric acid, chlorination
Hydrogen reaches experiment effect to the competitive reaction power difference of moisture, and wherein concentrated sulfuric acid water suction, hydrogen chloride gas are dissolved in
Water belongs to physical reactions.
Chlorosilane raffinate, which meets water, violent chemical reaction occurs, and is apparently higher than the concentrated sulfuric acid to the competitiveness of moisture, so that
Chlorosilane raffinate hydrolysis smoothly occurs.
The hydrogen chloride gas that chlorosilane raffinate generates when hydrolyzing is extremely difficult in concentrated sulfuric acid atmosphere to be dissolved in water, the competition to moisture
Power is less than the concentrated sulfuric acid, so that hydrogen chloride overflows in gaseous form.
HCl(g) + H2OH3O+ + Cl-
The reaction equation is the ionization equation that hydrogen chloride gas obtains hydrochloric acid solution in conjunction with water, and hydrogen chloride gas is dissolved in water
When scission of link formed into H3O+And Cl-, due to H in concentrated sulfuric acid solution3O+Content it is higher can inhibit hydrogen chloride gas scission of link formed H3O+And Cl-。
Beneficial effects of the present invention:
(1) H in the method for the invention2SO4It is not involved in chemical reaction and only embodies its water imbibition, therefore do not have to supplement
H2SO4Raw material has effect " once and for all ".
(2) hydrogen chloride that the method for the invention generates overflows purity in gaseous form and is up to 94%-97%, mentions by separation
The gas reclaiming rate obtained after pure hydrogen chloride at 85% or more, continuous hydrolysis can overflow in gaseous form always, can be efficient
Collect the hydrogen chloride gas of high quality.
(3) the method for the invention generates H that is simple for process, being collected into2Production of polysilicon can be directly returned with HCl
System achievees the purpose that chlorosilane raffinate resource utilization and zero-emission.
Detailed description of the invention
Fig. 1 is system structure diagram of the invention.
In Fig. 1: 1- stirred autoclave；2- Pulp pump；3- filter press；4- acid pump；5- sulfuric acid filtrate accumulator tank；6- condensation
Device；7- high-pressure separator.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawings and detailed description, but protection scope of the present invention is simultaneously
It is not limited to the content.
Equipment therefor of the embodiment of the present invention includes stirred autoclave 1, Pulp pump 2, filter press 3, acid pump 4, sulfuric acid filtrate time
Slot 5, condenser 6, high-pressure separator 7 are received, the upper end of stirred autoclave 1 is connected to chlorosilane raffinate storage device, and lower end passes through
Pulp pump 2 is connected to filter press 3, and filter press 3 is connected to sulfuric acid filtrate accumulator tank 5, and the lower end of sulfuric acid filtrate accumulator tank 5 passes through acid
Pump 4 is connected to stirred autoclave 1；Sulfuric acid filtrate accumulator tank 5, stirred autoclave 1 upper end be connected to condenser 6, condenser 6
Lower end be connected to stirred autoclave 1, condenser 6 is connected to high-pressure separator 7, as shown in Figure 1.
The main component mass percent of the chlorosilane raffinate of embodiment processing is 93% SiCl4, 4.8% SiHCl3、
2.1% SiH2Cl2, 0.1% other impurities.
Embodiment 1
A kind of method for producing gas phase chlorination hydrogen using chlorosilane raffinate, specifically includes following steps such as described in the present embodiment
Under: it is placed in stirred autoclave 1 using the sulfuric acid 1000g that the industrial concentrated sulfuric acid prepares 20%, 3200g chlorosilane raffinate is slowly added dropwise
And be stirred continuously, the mixed gas for reacting generation enters in condenser 6, adjusts the temperature of condenser at -15 DEG C, liquid condensed is simultaneously
Back to continuing to hydrolyze in stirred autoclave 1, gaseous substance enters in high-pressure separator 7, and the pressure for adjusting separator exists
2.4Mpa is collected the liquid that high-pressure separator is isolated using the resistance to demijohn of vacuum, while being collected and being divided using hydrogen storage
The hydrogen come is separated out, resistance to demijohn weight gain 2501.3g is weighed after collection, calculates and knows that the hydrogen chloride rate of recovery is 86.6%, through gas
It is 95.4% that body purity testing instrument, which detects its purity,.
The slurry on stirred autoclave top is extracted into filter press 3 by Pulp pump 2 and carries out filters pressing, filtrate enters sulfuric acid filtrate
In accumulator tank 5, industry water adjustment sulfuric acid concentration is supplemented into sulfuric acid filtrate accumulator tank 5 between 20%-60%, after peracid pump 4
It returns in stirred autoclave 1, carries out subsequent hydrolysis.
Embodiment 2
A kind of method for producing gas phase chlorination hydrogen using chlorosilane raffinate, specifically includes following steps such as described in the present embodiment
Under: it is placed in stirred autoclave 1 using the sulfuric acid 1000g that the industrial concentrated sulfuric acid prepares 40%, 2000g chlorosilane raffinate is slowly added dropwise
And be stirred continuously, the mixed gas for reacting generation enters in condenser 6, adjusts the temperature of condenser at -20 DEG C, liquid condensed is simultaneously
Back to continuing to hydrolyze in stirred autoclave 1, gaseous substance enters in high-pressure separator 7, and the pressure for adjusting separator exists
2.0Mpa is collected the liquid that high-pressure separator is isolated using the resistance to demijohn of vacuum, while being collected and being divided using hydrogen storage
The hydrogen come is separated out, resistance to demijohn weight gain 1572.4g is weighed after collection, calculates and knows that the hydrogen chloride rate of recovery is 87.1%, through gas
It is 96.1% that body purity testing instrument, which detects its purity,.
The slurry on stirred autoclave top is extracted into filter press 3 by Pulp pump 2 and carries out filters pressing, filtrate enters sulfuric acid filtrate
In accumulator tank 5, industry water adjustment sulfuric acid concentration is supplemented into sulfuric acid filtrate accumulator tank 5 between 20%-60%, after peracid pump 4
It returns in stirred autoclave 1, carries out subsequent hydrolysis.
Embodiment 3
A kind of method for producing gas phase chlorination hydrogen using chlorosilane raffinate, specifically includes following steps such as described in the present embodiment
Under: it is placed in stirred autoclave 1 using the sulfuric acid 1000g that the industrial concentrated sulfuric acid prepares 60%, 880g chlorosilane raffinate is slowly added dropwise simultaneously
It is stirred continuously, the mixed gas for reacting generation enters in condenser 6, adjusts the temperature of condenser at -30 DEG C, liquid condensed is simultaneously returned
It returning in stirred autoclave 1 and continues to hydrolyze, gaseous substance enters in high-pressure separator 7, adjust the pressure of separator in 2.2Mpa,
The liquid that high-pressure separator is isolated is collected using the resistance to demijohn of vacuum, while being separated using hydrogen storage collection
Hydrogen weighs resistance to demijohn weight gain 679.2g after collection, calculate and know that the hydrogen chloride rate of recovery is 85.5%, survey through gas purity
Determine instrument to detect its purity to be 94.3%.
The slurry on stirred autoclave top is extracted into filter press 3 by Pulp pump 2 and carries out filters pressing, filtrate enters sulfuric acid filtrate
In accumulator tank 5, industry water adjustment sulfuric acid concentration is supplemented into sulfuric acid filtrate accumulator tank 5 between 20%-60%, after peracid pump 4
It returns in stirred autoclave 1, carries out subsequent hydrolysis.
Claims (4)
1. a kind of method for producing gas phase chlorination hydrogen using chlorosilane raffinate, which is characterized in that specifically includes the following steps:
(1) sulfuric acid solution is placed in stirred autoclave (1), then chlorosilane raffinate is slowly dropped in sulfuric acid solution, no
Disconnected stirring is uniformly mixed reactant；
(2) being continuously added with chlorosilane raffinate, the gas generated in reaction kettle enter in condenser (6), the liquid being condensed out
Phase substance returns in stirred autoclave (1), and gaseous substance enters in high-pressure separator (7), to the liquid phase substance and gas isolated
Phase substance is recycled respectively, and liquefied hydrogen chloride becomes the hydrogen chloride of gas phase at normal temperatures and pressures；
(3) silicon dioxide colloid that hydrolysis generates floats because density is less than sulfuric acid, will be stirred to react by Pulp pump (2)
The slurry on kettle top is extracted into filter press (3) and carries out filters pressing, and filtrate enters industrial moisturizing adjustment sulfuric acid in sulfuric acid filtrate accumulator tank (5)
It is returned in stirred autoclave (1) after peracid pumps (4) after the concentration of filtrate；
The mass percent concentration of sulfuric acid solution described in step (1) is 20%-60%, the charging of chlorosilane raffinate and sulfuric acid solution
Mass ratio is 11:50-16:5.
2. the method according to claim 1 for producing gas phase chlorination hydrogen using chlorosilane raffinate, it is characterised in that: condenser
(6) temperature is -30 ~ -15 DEG C, and the liquefaction of gas phase chlorosilane raffinate is made to return to hydrolysis, hydrogen chloride gas and two kinds of substances of hydrogen with
Gas phase state enters high-pressure separator (7), controls the pressure of high-pressure separator (7) between 1.9 ~ 2.5Mpa, hydrogen chloride gas
Liquefaction and Hydrogen Separation come.
3. the method according to claim 1 for producing gas phase chlorination hydrogen using chlorosilane raffinate, it is characterised in that: stirring is anti-
Chlorosilane raffinate hydrolysis temperature in kettle (1) is answered to control between 20 DEG C -50 DEG C.
4. the method equipment therefor of gas phase chlorination hydrogen is produced described in claim 1 ~ 3 any one using chlorosilane raffinate, it is special
Sign is: including stirred autoclave (1), Pulp pump (2), filter press (3), acid pump (4), sulfuric acid filtrate accumulator tank (5), condenser
(6), the upper end of high-pressure separator (7), stirred autoclave (1) is connected to chlorosilane raffinate storage device, and lower end passes through Pulp pump
(2) it is connected to filter press (3), filter press (3) is connected to sulfuric acid filtrate accumulator tank (5), and the lower end of sulfuric acid filtrate accumulator tank (5) is logical
Peracid pump (4) is connected to stirred autoclave (1)；Sulfuric acid filtrate accumulator tank (5), stirred autoclave (1) upper end and condenser
(6) it is connected to, the lower end of condenser (6) is connected to stirred autoclave (1), and condenser (6) is connected to high-pressure separator (7).
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109650339A (en) * | 2019-01-16 | 2019-04-19 | 杭州东日节能技术有限公司 | Hydrolyzing chlorosilane prepares the technique and device of hydrogen chloride |
| CN114699894B (en) * | 2022-03-07 | 2023-06-20 | 中船(邯郸)派瑞特种气体股份有限公司 | Recovery device and method for residual gas in gas-liquid hydrolysis reaction |
| CN115646125B (en) * | 2022-11-08 | 2023-10-31 | 瑞燃(上海)环境工程技术有限公司 | System and method for purifying and recycling high-concentration hydrogen chloride tail gas |
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