CN217526448U - Organic silicon acid hydrolysate deacidification device - Google Patents
Organic silicon acid hydrolysate deacidification device Download PDFInfo
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- CN217526448U CN217526448U CN202221008543.4U CN202221008543U CN217526448U CN 217526448 U CN217526448 U CN 217526448U CN 202221008543 U CN202221008543 U CN 202221008543U CN 217526448 U CN217526448 U CN 217526448U
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Abstract
The utility model discloses an organic silicon acidic hydrolysate deacidification device, wherein the upper part of an extraction tower is provided with a process water inlet and a neutral hydrolysate outlet; the lower part of the extraction tower is provided with an acidic hydrolysate inlet and a hydrochloric acid outlet; the neutral hydrolysate outlet of the extraction tower is connected with the neutral hydrolysate tank, and the hydrochloric acid outlet is connected with the hydrochloric acid tank. And a regulating valve is arranged on a connecting pipeline at the hydrochloric acid outlet and is connected with an interface meter at the upper part of the extraction tower to form interlocking. Feeding process water from the upper part of the extraction tower, feeding acidic hydrolysate from the bottom of the extraction tower, and carrying out countercurrent contact on the process water and the acidic hydrolysate in the extraction tower, wherein qualified neutral hydrolysate is obtained at the top of the extraction tower, and dilute hydrochloric acid is obtained at the lower part of the extraction tower. The method has the advantages of simple process, high efficiency and less device investment, and can remove the chlorine in the acidic hydrolysate in one step to ensure that the chlorine content in the hydrolysate is less than 15ppm.
Description
Technical Field
The utility model relates to an organic silicon acidic hydrolysate dechlorination device, which belongs to the technical field of organic silicon production.
Background
The organic silicon material is a novel material developed in recent decades, mainly comprises four major classes of silicon rubber, silicon oil, a silane coupling agent and silicon resin, and is widely applied to the industries of aerospace, medical engineering, mechanical manufacturing and the like. The raw material for producing the organosilicon material is the polysiloxane obtained by hydrolyzing and cracking dimethyldichlorosilane.
With the progress of organic silicon production technology and the higher environmental protection requirement, the original commonly adopted constant boiling acid hydrolysis process of the dimethyldichlorosilane is replaced by an advanced gas phase hydrolysis process. Compared with the azeotropic acid hydrolysis process, although the pressurized synthesis of the gaseous phase hydrogen chloride and the chloromethane can be directly obtained by the gaseous phase hydrolysis, the cycle ratio of the hydrolysate is low, the viscosity is high, and the encapsulated chlorine is difficult to remove, so that the content of chloride ions in the hydrolysate is high. In the industry, a method of multistage kettle type stirring water washing and alkali washing is generally adopted for removing chlorine in hydrolysis, but chlorine wrapped in hydrolysate is difficult to disperse through stirring, so that the dechlorination process is long, the hydrolysate loss is large, and the wastewater amount is large.
The invention content is as follows:
to present technical problem, the utility model aims at providing a device of dechlorination of acid hydrolysate that the flow is simple, efficient accomplishes the desorption of chlorine in the acid hydrolysate in one step, directly obtains qualified neutral hydrolysate, and it is big with alkali-wash flow sewage volume to solve multistage washing in the current flow, and the problem of hydrolysate loss reduces the device investment, improves system operation efficiency.
A device for dechlorinating organic silicon acidic hydrolysate is characterized in that a process water inlet and a neutral hydrolysate outlet are formed in the upper part of an extraction tower; the lower part of the extraction tower is provided with an acidic hydrolysate inlet and a hydrochloric acid outlet; the neutral hydrolysate outlet of the extraction tower is connected with the neutral hydrolysate tank, and the hydrochloric acid outlet is connected with the hydrochloric acid tank.
And a regulating valve is arranged on a connecting pipeline at the hydrochloric acid outlet and is connected with an interface meter at the upper part of the extraction tower to form interlocking.
The extraction tower is internally provided with a rotating disc tower, and the theoretical grade of the rotating disc tower is 10-50 blocks, preferably 20-30 blocks. The material is made of materials which are resistant to hydrochloric acid corrosion, such as titanium, zirconium, polytetrafluoroethylene, hastelloy, graphite and the like.
The dechlorination process of the organic silicon acidic hydrolysate by adopting the device of the utility model comprises the following process steps:
the acidic hydrolysate from the previous loop is conveyed into an acidic hydrolysate inlet through a pump and is in reverse contact with the process water from the process water inlet in the extraction tower;
the two substances are in reverse contact mass transfer exchange, hydrogen chloride in the acidic hydrolysate is absorbed into water, the hydrogen chloride is regulated and extracted to a hydrochloric acid tank by an extraction tower kettle, the deacidified hydrolysate flows to the top of the extraction tower and overflows to a neutral hydrolysate tank, the interface height of the hydrolysate on the upper part of the extraction tower is controlled by controlling the extraction amount of the extraction tower kettle, the interface of an oil phase and a water phase is controlled in the middle of a top view mirror, and the hydrolysate can be ensured to normally overflow to the neutral hydrolysate tank. The two substances are in reverse contact mass transfer, hydrogen chloride in the acidic hydrolysate is absorbed into water, the hydrogen chloride flows to the extraction tower kettle due to high density, an upper oil-water interface is adjusted by an adjusting valve and is extracted to a hydrochloric acid tank, the concentration of hydrochloric acid in the hydrochloric acid tank is 5% -10%, and the hydrochloric acid returns to the previous hydrolysis loop for recycling. The deacidified hydrolysate has low density, flows to the top of the extraction tower, overflows to a neutral hydrolysate tank, and has a chlorine content of less than 15ppm. The working pressure of the extraction tower is normal pressure, and the working temperature is maintained at 60-90 ℃ by adopting engineering technical means. The rotating speed of the rotating disc is 90-150 revolutions per minute.
The acidic hydrolysate is prepared from cyclic siloxane ((CH) 3 ) 2 SiO) n (n =3 to 7 and n is an integer) and a linear siloxane HO ((CH) 3 ) 2 SiO) n H, (n = 3-10 and n is an integer), hydrochloric acid and unreacted methylchlorosilane monomer.
The neutral hydrolysate comprises cyclic siloxane ((CH) 3 ) 2 SiO) n And linear siloxane HO ((CH) 3 ) 2 SiO) n H。
The content of hydrochloric acid in the acidic hydrolysate is 1% -5%, and the mass ratio of the process water to the acidic hydrolysate is 1:3-5.
Adding a surfactant with the mass of 1-5% of that of the acidic hydrolysate from the previous loop before the acidic hydrolysate enters the bottom of the extraction tower to inhibit the acidic hydrolysate from being continuously crosslinked, controlling the viscosity of the acidic hydrolysate to be 30-50cp and controlling the viscosity of the neutral hydrolysate to be about 60cp, wherein the surfactant is an organic solvent with the boiling point of 80-150 ℃, preferably C4-C9 alkane or alcohols such as amyl alcohol, butanol, n-hexanol and the like, and the surfactant of the alkane has stable property, only plays a role in inhibiting the hydrolysate from being continuously hydrolyzed and crosslinked, does not participate in the reaction, has the boiling point of 80-150 ℃, and is convenient to separate from the hydrolysate.
The utility model discloses equipment is simple, and the investment economizes. The characteristic of large shearing force of the rotating disc of the extraction tower is utilized, acid chloride wrapped in hydrolysate is beneficial to breaking balance and entering a water phase, the efficiency is high, and the multistage tower type extraction is adopted to replace all subsequent loop hydrolysis energy levels. And no water washing wastewater and alkali washing wastewater are discharged, so that the hydrolysate loss caused by carrying the hydrolysate in the wastewater is reduced, and the method is environment-friendly and energy-saving. Meanwhile, by controlling the process parameters and adding the surfactant, the molecular weight range of the hydrolysate can be effectively controlled, and the quality of the hydrolysate is improved.
Drawings
FIG. 1 is a device for dechlorinating organic silicon acidic hydrolysate, 1. An extraction tower; 2. a neutral hydrolysate tank; 3. a hydrochloric acid tank; 4. adjusting a valve; 5. an interface meter; 1-1, a process water inlet; 1-2, importing an acidic hydrolysate; 1-3, a neutral hydrolysate outlet; 1-4, hydrochloric acid outlet; 6. a rotating disc tower.
Detailed Description
The invention will be further described with reference to the accompanying drawings and specific embodiments, but the scope of the invention is not limited thereto.
Example 1
A device for dechlorinating organic silicon acidic hydrolysate is characterized in that a process water inlet 1-1 and a neutral hydrolysate outlet 1-3 are arranged at the upper part of an extraction tower 1; the lower part of the extraction tower 1 is provided with an acidic hydrolysate inlet 1-2 and a hydrochloric acid outlet 1-4; neutral hydrolysate outlets 1-3 of the extraction tower 1 are connected with a neutral hydrolysate tank 2, and hydrochloric acid outlets 1-4 are connected with a hydrochloric acid tank 3.
The connecting pipeline at the hydrochloric acid outlet 1-4 is provided with a regulating valve 4, and the regulating valve 4 is connected with an interface meter 5 at the upper part of the extraction tower 1 and forms interlocking.
The inside carousel tower 6 that sets up of extraction tower 1, theoretical level 25, 6 barrel materials steel lining tetrafluoros of carousel tower, pivot material are the tetrafluoro spraying, and the carousel material is the tetrafluoro package steel.
Example 2
The acidic hydrolyzate in this example was prepared from cyclic siloxane ((CH) 3 ) 2 SiO) n (n =3 to 7 and n is an integer) and a linear siloxane HO ((CH) 3 ) 2 SiO) n H, (n = 3-10 and n is an integer), hydrochloric acid and unreacted methylchlorosilane monomer.
The neutral hydrolysate comprises cyclic siloxane ((CH) 3 ) 2 SiO) n And linear silicones HO ((CH) 3 ) 2 SiO) n H。
The acid hydrolysate from the dilute acid dimethyl dichlorosilane hydrolysis loop, with a hydrochloric acid content of 2%, was pumped to the bottom of the extraction column and contacted countercurrently with process water in the extraction column. The mass ratio of the process water to the acidic hydrolysate is 1:4. the two substances are in reverse contact mass transfer, the concentration of hydrochloric acid obtained at the bottom of the extraction tower is about 5 percent, and the hydrochloric acid enters a hydrochloric acid tank and returns to a concentrated acid hydrolysis loop for recycling. The hydrolysate at the upper part of the extraction tower overflows to a neutral hydrolysate tank, the chlorine content in the hydrolysate is 10ppm and the viscosity of the neutral hydrolysate is 51cp. In the process, the height of a hydrolysate interface at the upper part of an extraction tower is controlled by controlling the extraction amount of an extraction tower kettle, and an oil-water phase interface is controlled to be positioned in the middle of a top sight glass. The working pressure of the extraction tower is normal pressure, and the working temperature is maintained at 70 ℃ by taking a heat preservation measure of a preheating meter for feeding materials. The extraction column rotating disc rotating speed is 100 r/min.
Claims (3)
1. An organic silicon acidic hydrolysate deacidification device is characterized in that a process water inlet (1-1) and a neutral hydrolysate outlet (1-3) are arranged at the upper part of an extraction tower (1); the lower part of the extraction tower (1) is provided with an acidic hydrolysate inlet (1-2) and a hydrochloric acid outlet (1-4); neutral hydrolysate outlets (1-3) of the extraction tower (1) are connected with the neutral hydrolysate tank (2), and hydrochloric acid outlets (1-4) are connected with the hydrochloric acid tank (3).
2. The deacidification plant for organosilicon acidic hydrolysates according to claim 1, characterized in that the connecting lines at the hydrochloric acid outlets (1-4) are provided with regulating valves (4), and the regulating valves (4) are connected with an interface meter (5) at the upper part of the extraction column (1) and form an interlock.
3. The deacidification plant for organosilicon acidic hydrolysates according to claim 1, characterized in that a rotating tray tower (6) is arranged inside the extraction tower (1), the theoretical stage of the rotating tray tower (6) being 10-50 blocks.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114949923A (en) * | 2022-04-28 | 2022-08-30 | 湖北兴瑞硅材料有限公司 | Method and device for deacidifying organic silicon acidic hydrolysate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114949923A (en) * | 2022-04-28 | 2022-08-30 | 湖北兴瑞硅材料有限公司 | Method and device for deacidifying organic silicon acidic hydrolysate |
| CN114949923B (en) * | 2022-04-28 | 2023-11-10 | 湖北兴瑞硅材料有限公司 | Method and device for deacidifying organosilicate hydrolysate |
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