An inert high-boiling silicone oil production line and its production process
The hydrolysis, dechlorination, dehydrogenation-neutralization, and polymerization reaction units of the inert high-boiling silicone oil production line have solved the problem of treating high-boiling-point silicones, producing high-quality high-boiling silicone oils suitable for silicone coatings and silicone rubbers. This solves the problems of difficult reaction control and product instability in existing technologies.
Patent Information
- Application Number
- CN202310891996.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-07-19
- Publication Date
- 2025-12-02
- Estimated Expiration
- 2043-07-19
AI Technical Summary
Existing technologies are ineffective in treating high-boiling-point organosilicon compounds, leading to environmental pollution and production difficulties. Furthermore, existing methods for preparing high-boiling-point silicone oils suffer from problems such as uncontrollable reactions and unstable product performance.
An inert high-boiling silicone oil production line is adopted, including hydrolysis, dechlorination, dehydrogenation-neutralization and polymerization reaction units. Inert high-boiling silicone oil is prepared by hydrolysis reaction of concentrated hydrochloric acid with high-boiling substances, combined with treatment of activated clay, catalyst and solid acid molecular sieve.
The production process of high-boiling silicone oil is simple and controllable, and the product performance is stable. It is suitable for the production of organosilicon coatings and silicone rubber, and produces high-quality high-boiling silicone oil with low chloride ions and no hydrogen.
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Figure CN116920745B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of silicone oil preparation technology, specifically relating to an inert high-boiling silicone oil production line and its production process. Background Technology
[0002] In recent years, with the rapid development of the domestic organosilicon industry, the output of organosilicon monomers, such as methylchlorosilanes, has been increasing. Consequently, the amount of organosilicon high-boiling-point byproducts generated during the synthesis of organosilicon monomers has also increased. Statistics show that the current domestic organosilicon monomer production capacity has reached 8 million tons per year, and the output of high-boiling-point byproducts, which account for approximately 3% to 5% of the total monomer production, will reach 200,000 to 400,000 tons. The composition of high-boiling-point organosilicon compounds is extremely complex, mainly consisting of Si-Si, Si-C-Si, and Si-O-Si bond structures. They have a normal pressure density of approximately 1.13 g / ml, a boiling range of 80–215℃, and contain a large amount of solid particulate impurities such as silicon powder and copper catalysts. They appear as a brown or yellow liquid and readily react with moisture in the air to generate corrosive hydrogen chloride gas. This makes it impossible to treat high-boiling-point organosilicon compounds using simple methods, classifying them as hazardous chemical waste. If these high-boiling-point organosilicon byproducts are not treated promptly and effectively, they will inevitably have a severe impact on the environment, thereby affecting the normal production of organosilicon monomer manufacturers. Currently, this has become a prominent problem faced by organosilicon monomer production enterprises.
[0003] However, the applications of high-boiling-point organosilicon compounds are limited. Currently, the main methods for the comprehensive utilization of high-boiling-point organosilicon compounds include the cracking method for producing monosilanes and the alcoholysis / hydrolysis method for producing high-boiling-point silicone oil. The cracking of high-boiling-point organosilicon compounds generally involves breaking them down into useful monomers such as dimethyldichlorosilane under high temperature and high pressure conditions in the presence of different raw materials, as illustrated by the technical solutions disclosed in Chinese patents with publication numbers CN101298051A and CN1590389A. Furthermore, the preparation of high-boiling-point silicone oils through alcoholysis / hydrolysis of high-boiling-point organosilicon compounds has advantages such as simple process, low cost, and ease of industrialization, and has become one of the research hotspots for the utilization of high-boiling-point organosilicon compounds, as illustrated by the technical solutions disclosed in Chinese patents with publication numbers CN101016383B and CN112142975B. However, existing reported technologies all suffer from varying degrees of problems, including difficulty in controlling the reaction, complex processes, and unstable product performance. For example, the pyrolysis reaction of high-boiling-point organosilicon compounds is difficult to control, resulting in low dimethylchlorosilane content, low conversion rate, difficulty in separating monomers after pyrolysis, and high cost. The alcoholysis method for preparing high-boiling-point silicone oil is prone to product neutralization difficulties and acid reversion. Similarly, the hydrolysis method also suffers from acid reversion and excessively high volatile content in the prepared high-boiling-point silicone oil. Furthermore, existing technologies for preparing high-boiling-point silicone oil from high-boiling-point organosilicon compounds, such as alcoholysis / hydrolysis, yield silicone oil with alkoxy-active functional groups, which can only be used for treating dry powder fire extinguishing agents and cannot be used for the preparation of room-temperature curing silicone rubber.
[0004] Therefore, developing effective technologies for the production and utilization of high-boiling-point organosilicon compounds and alleviating the problem of by-product treatment in organosilicon monomer production is of great significance to the healthy and circular development of the organosilicon monomer industry. Summary of the Invention
[0005] The purpose of this invention is to address the aforementioned technical problems by providing an inert high-boiling silicone oil production line and its production process, in order to prepare an inert high-boiling silicone oil without active groups, making it suitable for the production of organosilicon coatings, silicone rubber, etc., while making the production and preparation process of high-boiling silicone oil simple, controllable, and the product performance stable.
[0006] In view of this, the present invention provides a production line for inert high-boiling silicone oil, comprising:
[0007] A hydrolysis reaction unit, comprising a reaction tower, wherein concentrated hydrochloric acid and a high-boiling-point substance are introduced into the reaction tower to carry out a hydrolysis reaction;
[0008] A dechlorination reaction unit includes a dechlorination reactor, into which oil phase substances discharged from the reaction tower enter and undergo a dechlorination reaction to remove unhydrolyzed chlorine;
[0009] A dehydrogenation-neutralization reaction unit includes a dehydrogenation-neutralization reactor, wherein oil phase substances discharged from the dechlorination reactor enter the dehydrogenation-neutralization reactor to carry out dehydrogenation and neutralization reactions;
[0010] A polymerization reaction unit includes a polymerization reactor, into which oil phase substances discharged from the dehydrogenation-neutralization reactor enter and undergo polymerization reaction;
[0011] The oil phase material discharged from the polymerization reactor enters the evaporation unit, and after evaporation to remove low-component substances, an inert high-boiling silicone oil product is obtained.
[0012] Furthermore, the hydrolysis reaction unit also includes:
[0013] The pre-reactor has its feed end connected to the aqueous phase outlet located in the bottom of the reaction tower, and its discharge end connected to the feed inlet located at the top of the reaction tower.
[0014] Concentrated hydrochloric acid and high-boiling substances are first mixed and pre-reacted in the pre-reactor, and then enter the reaction tower for a complete hydrolysis reaction.
[0015] Furthermore, the hydrolysis reaction unit also includes:
[0016] A heat exchanger, located between the reaction tower and the pre-reactor, is used to cool the material discharged from the aqueous phase outlet of the reaction tower bottom.
[0017] A circulating pump, located between the heat exchanger and the reaction tower, is used to pump the material discharged from the aqueous phase outlet of the reaction tower into the heat exchanger.
[0018] Furthermore, the pre-reactor includes a pre-reactor front section and a pre-reactor rear section:
[0019] A Venturi tube is installed at the front end of the pre-reactor. Hydrochloric acid enters the pre-reactor from the inlet of the Venturi tube. At the same time, a negative pressure is generated at the throat of the Venturi tube. Under the action of this negative pressure, high-boiling substances are drawn into the Venturi tube.
[0020] A material mixing structure is provided in the rear section of the pre-reactor. The material mixing structure includes multiple baffles arranged alternately in the rear section of the pre-reactor, and the baffles form a serpentine material channel in the rear section of the pre-reactor.
[0021] Furthermore, the reaction tower is divided into an upper section and a lower section, with a swirling structure installed in the upper section and a lower cavity formed in the lower section.
[0022] Furthermore, the hydrolysis reaction unit also includes:
[0023] The first intermediate tank is connected to the oil phase outlet of the reaction tower.
[0024] The oil phase produced by the hydrolysis reaction of concentrated hydrochloric acid and high-boiling substances flows into the first intermediate tank through the oil phase outlet. The material entering the first intermediate tank undergoes oil-water separation. The separated oil phase overflows from the top of the first intermediate tank into the dechlorination reactor, while the water phase returns from the bottom of the first intermediate tank to the reaction tower.
[0025] Furthermore, the dechlorination reactor includes: an upper section of the dechlorination reactor, a middle section of the dechlorination reactor, and a lower section of the dechlorination reactor;
[0026] A first filtration structure is provided in the upper section of the dechlorination reactor, and the first filtration structure is located in the lower part of the upper section of the dechlorination reactor;
[0027] A heating structure is provided in the middle section of the dechlorination reactor;
[0028] The dechlorination reactor has a feed inlet at the top of the lower section and a by-product discharge outlet at the bottom.
[0029] Furthermore, the dechlorination reaction unit also includes:
[0030] The activated clay and the HCl produced by its adsorption and neutralization enter the lower section of the dechlorination reactor. After settling, the filtrate enters the centrifuge from the bottom of the dechlorination reactor. After filtration by the centrifuge, the filtrate is returned to the dechlorination reactor for reuse.
[0031] Furthermore, the dehydrogenation-neutralization reactor includes: an upper section of the dehydrogenation-neutralization reactor, a middle section of the dehydrogenation-neutralization reactor, and a lower section of the dehydrogenation-neutralization reactor;
[0032] The dehydrogenation-neutralization reactor is equipped with sintered nickel chloride adsorption packing and heating structure in the middle section;
[0033] The sum of the volumes of the upper and lower sections of the dehydrogenation-neutralization reactor is 30-50% of the volume of the middle section of the dehydrogenation-neutralization reactor.
[0034] Furthermore, the top of the tunable polymerization reactor is a vent, a discharge port is provided on the side near the top, and a feed port is provided at the bottom. The top and bottom of the tunable polymerization reactor are respectively provided with a second filter structure, and a heating structure is provided in the second filter structure to maintain the temperature of the second filter structure at 80-100°C.
[0035] Furthermore, the evaporation unit includes:
[0036] In the thin-film evaporator, the oil phase material discharged from the polymer reactor is subjected to vacuum de-lowering treatment to remove low-component substances.
[0037] Furthermore, the evaporation unit also includes:
[0038] The seventh intermediate tank is connected to the low-component material outlet on the thin-film evaporator. The low-component material removed by the vacuum de-lowering process is condensed and stored in the seventh intermediate tank.
[0039] The sixth transfer pump is connected to the seventh intermediate tank and the polymerization reactor respectively, and is used to transport and reuse the material in the seventh intermediate tank to the polymerization reactor.
[0040] A production process for inert high-boiling-point silicone oil, wherein the production process uses the above-mentioned production line to prepare inert high-boiling-point silicone oil, and the production process includes the following steps:
[0041] S1, concentrated hydrochloric acid and high-boiling substances undergo hydrolysis reaction in the reaction tower;
[0042] S2, the oil phase material after hydrolysis reaction reacts with activated clay in the dechlorination reactor to remove the unhydrolyzed chlorine;
[0043] S3, the oil phase material after the dechlorination reaction enters the dehydrogenation-neutralization reactor, where hydrogen is removed under the action of a catalyst, and at the same time, it undergoes a neutralization reaction with alkaline water;
[0044] S4, the oil phase material after the dehydrogenation-neutralization reaction enters the polymerization reactor and undergoes polymerization under the action of solid acid molecular sieve;
[0045] S5, after the polymerization reaction, the oil phase material is subjected to vacuum de-lowering treatment to remove low-component substances, resulting in an inert high-boiling silicone oil product.
[0046] Furthermore, in step S1, the mass concentration of concentrated hydrochloric acid is 25-30%; the flow ratio of concentrated hydrochloric acid to high-boiling-point substance is 50-100:1; the method of adding concentrated hydrochloric acid and high-boiling-point substance is as follows: first, concentrated hydrochloric acid is added to the lower chamber of the reaction tower, and the liquid level of concentrated hydrochloric acid is controlled to be lower than the oil phase outlet of the reaction tower. Then, the circulation pump is turned on, and the concentrated hydrochloric acid is cooled by the heat exchanger and pumped into the pre-reactor. The concentrated hydrochloric acid enters from the inlet of the venturi tube, and at the same time, the high-boiling-point substance is drawn in from the throat on the side of the venturi tube.
[0047] Furthermore, in step S1, the residence time of the oil phase substance in the reaction tower is controlled to be 1 to 3 hours.
[0048] Furthermore, in step S2, the amount of activated clay used is 1-5% of the mass of the oil phase material; the temperature in the middle section of the dechlorination reactor is 70-100°C, and the residence time of the oil phase material in the middle section of the dechlorination reactor is 2-4 hours.
[0049] Furthermore, in step S3, the alkaline solution is one or more of sodium carbonate solution, sodium bicarbonate solution, or ammonia solution.
[0050] Furthermore, in step S3, the temperature in the middle section of the dehydrogenation-neutralization reactor is maintained at 80-100°C, and the residence time of the material in the middle section of the dehydrogenation-neutralization reactor is 2-4 hours.
[0051] Furthermore, in step S4, the residence time of the oil phase material in the heating section of the polymer reactor is 1 to 2 hours.
[0052] The production line and process for the inert high-boiling silicone oil described in this invention have the advantages of simple and controllable production process, and suitability for continuous industrial production. It can produce high-quality high-boiling silicone oil with low chloride ion content, no hydrogen content, and controllable viscosity. Attached Figure Description
[0053] Figure 1 This is a schematic diagram of the structure of the inert high-boiling silicone oil production line described in this invention;
[0054] The markings in the diagram are as follows:
[0055] 1. Reaction tower; 101. Swirl structure; 102. Lower chamber; 103. Oil phase outlet; 2. Circulating pump; 3. Heat exchanger; 4. Pre-reactor; 401. Venturi tube; 402. Material mixing structure; 5. First intermediate tank; 6. First transfer pump; 7. Dechlorination reactor; 701. Upper section of dechlorination reactor; 702. Middle section of dechlorination reactor; 703. Lower section of dechlorination reactor; 8. Centrifuge; 9. Second intermediate tank; 10. Second transfer pump; 11. Third... 12. Intermediate Tank; 13. Fourth Intermediate Tank; 14. Third Transfer Pump; 15. Dehydrogenation-Neutralization Reactor; 16. Upper Section of Dehydrogenation-Neutralization Reactor; 17. Middle Section of Dehydrogenation-Neutralization Reactor; 18. Lower Section of Dehydrogenation-Neutralization Reactor; 19. Alkali Tank; 20. Fifth Intermediate Tank; 21. Fifth Transfer Pump; 22. Thin Film Evaporator; 23. Sixth Transfer Pump; 24. Seventh Intermediate Tank. Detailed Implementation
[0056] The technical solutions of the embodiments of this application will be clearly described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of this application. All other embodiments obtained by those skilled in the art based on the embodiments of this application are within the scope of protection of this application.
[0057] In the description of this application, it should be noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the exemplary embodiments according to this application. For ease of description, the dimensions of the various parts shown in the drawings are not drawn to actual scale. Techniques, methods, and devices known to those skilled in the art may not be discussed in detail, but where appropriate, such techniques, methods, and devices should be considered part of the specification. In all examples shown and discussed herein, any specific values should be interpreted as merely exemplary and not as limitations. Therefore, other examples of exemplary embodiments may have different values. It should be noted that similar reference numerals and letters in the following drawings denote similar items; therefore, once an item is defined in one drawing, it need not be further discussed in subsequent drawings.
[0058] It should be noted that the terms "first," "second," etc., used in the specification and claims of this application are used to distinguish similar objects and not to describe a specific order or sequence. It should be understood that such use of data can be interchanged where appropriate so that embodiments of this application can be implemented in orders other than those illustrated or described herein, and the objects distinguished by "first," "second," etc., are generally of the same class and are not limited in number; for example, a first object can be one or more. Furthermore, in the specification and claims, "and / or" indicates at least one of the connected objects, and the character " / " generally indicates that the preceding and following objects are in an "or" relationship.
[0059] It should be noted that in the description of this application, the directional terms such as "front, back, up, down, left, right", "horizontal, vertical, horizontal" and "top, bottom" indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this application and simplifying the description. Unless otherwise stated, these directional terms do not indicate or imply that the device or element referred to must have a specific orientation or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation on the scope of protection of this application. The directional terms "inner" and "outer" refer to the inner and outer contours relative to the outline of each component itself.
[0060] It should be noted that, in this application, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Without further limitations, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes that element. Furthermore, it should be noted that the scope of the methods and apparatuses in the embodiments of this application is not limited to performing functions in the order shown or discussed, but may also include performing functions substantially simultaneously or in the reverse order, depending on the functions involved. For example, the described methods may be performed in a different order than described, and various steps may be added, omitted, or combined. Additionally, features described with reference to certain examples may be combined in other examples.
[0061] like Figure 1 As shown, a production line for an inert high-boiling silicone oil includes the following components arranged sequentially:
[0062] The hydrolysis reaction unit includes a reaction tower 1, in which concentrated hydrochloric acid and a high-boiling substance are first introduced into the reaction tower 1 to carry out the hydrolysis reaction.
[0063] The dechlorination reaction unit includes a dechlorination reactor 7, in which oil phase substances discharged from the reaction tower 1 enter the dechlorination reactor 7 and react with activated clay to remove unhydrolyzed chlorine (Si-Cl).
[0064] The dehydrogenation-neutralization reaction unit includes a dehydrogenation-neutralization reactor 14. Oil phase substances discharged from the dechlorination reactor 7 enter the dehydrogenation-neutralization reactor 14, where hydrogen (Si-H) is removed under the action of a catalyst; at the same time, a neutralization reaction occurs with alkaline water.
[0065] The polymerization reaction unit includes a polymerization reactor 18, which is equipped with a solid acid molecular sieve. Oil phase substances discharged from the dehydrogenation-neutralization reactor 14 enter the polymerization reactor 18 and undergo polymerization reaction under the action of the solid acid molecular sieve.
[0066] The oil phase material discharged from the polymerization reactor 18 enters the evaporation unit. After evaporation to remove low-component substances, an inert high-boiling silicone oil product is obtained.
[0067] Furthermore, the hydrolysis reaction unit also includes:
[0068] The pre-reactor 4 has its feed end connected to the aqueous phase outlet located in the bottom of the reaction tower 1, and its discharge end connected to the feed inlet located at the top of the reaction tower 1.
[0069] Concentrated hydrochloric acid and high-boiling substances are first mixed and pre-reacted in the pre-reactor 4, and then enter the reaction tower 1 through the feed port located at the top of the reaction tower 1, where a complete hydrolysis reaction is carried out.
[0070] Furthermore, the hydrolysis reaction unit also includes:
[0071] Heat exchanger 3, located between the reaction tower 1 and the pre-reactor 4, is used to cool the material discharged from the water phase outlet of the reactor 1, thereby regulating the temperature of the material entering the pre-reactor 4.
[0072] A circulating pump 2, located between the heat exchanger 3 and the reaction tower 1, is used to pump the material discharged from the aqueous phase outlet of the bottom of the reaction tower 1 into the heat exchanger 3.
[0073] Preferably, the pre-reactor 4 is a tubular reactor.
[0074] Furthermore, the pre-reactor 4 includes a pre-reactor front section and a pre-reactor rear section:
[0075] A Venturi tube 401 is installed at the front end of the pre-reactor. Hydrochloric acid enters the pre-reactor 4 from the inlet of the Venturi tube 401. At the same time, a negative pressure is generated at the throat of the Venturi tube 401. Under the action of this negative pressure, high-boiling substances are drawn into the Venturi tube 401, enter the front end of the pre-reactor, and mix with hydrochloric acid.
[0076] A material mixing structure 402 is provided in the rear section of the pre-reactor. The material mixing structure 402 includes multiple baffles arranged alternately in the rear section of the pre-reactor. The baffles form a serpentine material channel in the rear section of the pre-reactor, so that the concentrated hydrochloric acid and high-boiling substances flowing through it can fully mix and undergo pre-reaction.
[0077] Preferably, the baffle is arranged perpendicular to the central axis of the pre-reactor 4.
[0078] Furthermore, the reaction tower 1 can be divided into an upper section and a lower section. A swirling structure 101 is provided in the upper section of the reaction tower. The material entering the reaction tower 1 from the pre-reactor 4 can be further mixed and homogenized under the action of the swirling structure 101, which is conducive to the uniform distribution of the material in the reaction tower 1 and the synchronous and uniform reaction. At the same time, the material flows from the top of the reaction tower 1 to the lower part of the reaction tower 1 in a swirling manner, which is conducive to the timely discharge of hydrogen chloride generated by the reaction. Meanwhile, a lower cavity 102 is formed in the lower section of the reaction tower.
[0079] In addition, a hydrogen chloride gas exhaust port is provided at the top of the reaction tower 1, and an oil phase outlet 103 is provided in the middle of the reaction tower 1, through which the hydrolyzed oil phase material is discharged.
[0080] Furthermore, the hydrolysis reaction unit also includes:
[0081] First intermediate tank 5, the oil phase outlet 103 is connected to the first intermediate tank 5;
[0082] The oil phase produced by the hydrolysis reaction of concentrated hydrochloric acid and high-boiling substances flows into the first intermediate tank 5 through the oil phase outlet 103, the gas phase is discharged from the top of the reaction tower 1, and the aqueous phase is discharged through the aqueous phase outlet located at the bottom of the reaction tower 1.
[0083] Preferably, the material discharged from the reaction tower 1 enters the first intermediate tank 5 from the upper side of the first intermediate tank 5. The material entering the first intermediate tank 5 can undergo further oil-water separation therein. The separated oil phase overflows from the top of the first intermediate tank 5 into the dechlorination reactor 7, and the water phase returns from the bottom of the first intermediate tank 5 to the reaction tower 1.
[0084] As some embodiments of this application, the aqueous phase material discharged from the bottom of the first intermediate tank 5 and the material discharged from the aqueous phase outlet of the reactor 1 first enter the circulating pump 2, and then pass through the heat exchanger 3 and the pre-reactor 4. After being mixed with high-boiling substances in the pre-reactor 4, they enter the reactor 1.
[0085] Furthermore, the dechlorination reactor 7 includes: an upper section 701, a middle section 702, and a lower section 703.
[0086] A first filtration structure is provided in the upper section 701 of the dechlorination reactor, and the first filtration structure is located in the lower part of the upper section 701 of the dechlorination reactor;
[0087] The middle section 702 of the dechlorination reactor is equipped with a heating structure, and the temperature of the middle section 702 of the dechlorination reactor is controlled between 70 and 100°C by the heating structure.
[0088] The lower section 703 of the dechlorination reactor has a feed inlet at the top and a by-product discharge outlet at the bottom.
[0089] Preferably, the volume of the lower section 703 of the dechlorination reactor is 30-50% of the volume of the middle section 702 of the dechlorination reactor.
[0090] Furthermore, activated clay enters the dechlorination reactor 7 from below the first filter structure in the upper section 701 of the dechlorination reactor;
[0091] The oil phase material discharged from the hydrolysis reaction unit enters the dechlorination reactor 7 through the feed inlet located at the top of the lower section 703 of the dechlorination reactor. It undergoes a dechlorination reaction with activated clay in the middle section 702 of the dechlorination reactor to remove unhydrolyzed chlorine (Si-Cl). After the dechlorination reaction, the activated clay and the HCl and other substances produced by its adsorption and neutralization are discharged from the by-product discharge port at the bottom of the lower section 703 of the dechlorination reactor. The oil phase is filtered by the first filter structure in the upper section 701 of the dechlorination reactor and then discharged through the oil phase discharge port located on the top side of the upper section 701 of the dechlorination reactor. The gas generated by the reaction is discharged through the vent at the top of the dechlorination reactor 7.
[0092] Furthermore, the dechlorination reaction unit also includes:
[0093] Centrifuge 8, activated clay and the HCl produced by its adsorption and neutralization enter the lower section 703 of the dechlorination reactor. After settling, the filtrate enters the centrifuge 8 from the bottom of the dechlorination reactor 7. After being filtered by the centrifuge 8, the filtrate is returned to the dechlorination reactor 7 for reuse.
[0094] Specifically, the dechlorination reaction unit further includes:
[0095] The first transfer pump 6, the second intermediate tank 9, the second transfer pump 10, the third intermediate tank 11, and the fourth intermediate tank 12, wherein:
[0096] The first transfer pump 6 is located between the first intermediate tank 5 and the dechlorination reactor 7, and is used to pump the oil phase material in the first intermediate tank 5 to the dechlorination reactor 7;
[0097] The second intermediate tank 9 is connected to the filtrate discharge port of the centrifuge 8 and is used to store the filtrate discharged by the centrifuge 8;
[0098] The second transfer pump 10 is connected to the second intermediate tank 9 and the dechlorination reactor 7, and is used to pump the filtrate in the second intermediate tank 9 to the dechlorination reactor 7;
[0099] The third intermediate tank 11 is connected to the oil phase discharge port located in the upper section 701 of the dechlorination reactor and is used to store the oil phase substances discharged from the dechlorination reactor 7.
[0100] The fourth intermediate tank 12 is connected to the lower part of the upper section 701 of the dechlorination reactor. The fourth intermediate tank 12 stores activated clay and is used to transport the activated clay to the lower side of the filter structure in the upper section 701 of the dechlorination reactor.
[0101] Furthermore, the dehydrogenation-neutralization reactor 14 includes:
[0102] The upper section 1401 of the dehydrogenation-neutralization reactor, the middle section 1402 of the dehydrogenation-neutralization reactor, and the lower section 1403 of the dehydrogenation-neutralization reactor;
[0103] The top of the upper section 1401 of the dehydrogenation-neutralization reactor is a vent, the upper side is provided with the dehydrogenation-neutralization reactor outlet, and the bottom is provided with an alkaline water inlet;
[0104] The dehydrogenation-neutralization reactor middle section 1402 is equipped with sintered nickel chloride adsorption packing. The upper part of the lower section 1403 of the dehydrogenation-neutralization reactor is equipped with an oil phase inlet and the lower part is equipped with a water phase outlet. The dehydrogenation-neutralization reactor middle section 1402 is equipped with a heating structure to maintain the temperature of the dehydrogenation-neutralization reactor middle section 1402 between 80 and 100°C.
[0105] The oil phase discharged from the dechlorination reaction unit enters the dehydrogenation-neutralization reactor 14 through the oil phase inlet at the top of the lower section 1403 of the dehydrogenation-neutralization reactor. Then, in the middle section 1402 of the dehydrogenation-neutralization reactor, under the action of nickel chloride catalyst loaded on the packing and high temperature, hydrogen (Si-H) is removed. The gas generated by the dehydrogenation-neutralization reaction is discharged through the vent at the top of the dehydrogenation-neutralization reactor 14, the oil phase is discharged through the dehydrogenation-neutralization reactor outlet located on the upper side of the upper section 1401 of the dehydrogenation-neutralization reactor, and the aqueous phase is discharged through the aqueous phase outlet at the bottom of the lower section 1403 of the dehydrogenation-neutralization reactor and discharged after wastewater treatment.
[0106] Furthermore, the sum of the volumes of the upper section 1401 and the lower section 1403 of the dehydrogenation-neutralization reactor is 30 to 50% of the volume of the middle section 1402 of the dehydrogenation-neutralization reactor.
[0107] Furthermore, the dehydrogenation-neutralization reaction unit also includes:
[0108] The third transfer pump 13 is disposed between the third intermediate tank 11 and the dehydrogenation-neutralization reactor 14, and is used to pump the material in the third intermediate tank 11 to the dehydrogenation-neutralization reactor 14;
[0109] Alkali tank 15, which is connected to the alkali inlet at the bottom of the upper section 1401 of the dehydrogenation-neutralization reactor, is used to inject alkali into the dehydrogenation-neutralization reactor 14.
[0110] The fifth intermediate tank 16 is connected to the discharge port of the dehydrogenation-neutralization reactor provided on the upper side of the upper section 1401 of the dehydrogenation-neutralization reactor. The oil phase in the dehydrogenation-neutralization reactor 14 flows into the fifth intermediate tank 16 through the discharge port of the dehydrogenation-neutralization reactor provided on the upper side of the upper section 1401 of the dehydrogenation-neutralization reactor.
[0111] Furthermore, the top of the tunable polymerization reactor 18 is an vent, a discharge port is provided on the side near the top, and a feed port is provided at the bottom. The top and bottom of the tunable polymerization reactor 18 are respectively provided with a second filter structure, and a heating structure is provided in the second filter structure. The heating structure is used to maintain the temperature of the second filter structure at 80-100°C.
[0112] Furthermore, the telomerization reaction also includes:
[0113] The fourth transfer pump 17 is disposed between the fifth intermediate tank 16 and the polymerization reactor 18, and is used to pump the material in the fifth intermediate tank 16 to the polymerization reactor 18.
[0114] The sixth intermediate tank 19 is connected to the discharge port of the polymerization reactor 18 and is used to store the oil phase discharged from the polymerization reactor 18.
[0115] Furthermore, the evaporation unit includes:
[0116] In the thin-film evaporator 21, the oil phase material discharged from the polymer reactor 18 is subjected to vacuum de-lowering treatment to remove low-component substances.
[0117] Specifically, a feed inlet and a low-component material outlet are provided at the upper part of the thin-film evaporator 21, and a finished silicone oil outlet is provided at the bottom of the thin-film evaporator 21.
[0118] Furthermore, the evaporation unit also includes:
[0119] The fifth transfer pump 20 is located between the sixth intermediate tank 19 and the thin film evaporator 21, and is used to pump the material in the sixth intermediate tank 19 to the thin film evaporator 21;
[0120] The seventh intermediate tank 23 is connected to the low component material outlet on the thin film evaporator 21. The low component material removed by vacuum de-lowering treatment is condensed and stored in the seventh intermediate tank 23.
[0121] The sixth transfer pump 22 is connected to the seventh intermediate tank 23 and the polymerization reactor 18 respectively, and is used to transport and reuse the material in the seventh intermediate tank 23 to the polymerization reactor 18.
[0122] Preferably, the upper part of the seventh intermediate tank 23 is connected to the low component material outlet of the thin film evaporator 21, and the lower part is connected to the sixth transfer pump 22, which can transport the material in the seventh intermediate tank 23 to the bottom of the polymer reactor 18.
[0123] In addition, this application also provides a production process for inert high-boiling silicone oil, which includes the following steps:
[0124] S1, concentrated hydrochloric acid and high-boiling substances undergo hydrolysis reaction in reaction tower 1;
[0125] S2, the oil phase material after hydrolysis reaction reacts with activated clay in dechlorination reactor 7 to remove unhydrolyzed chlorine (Si-Cl).
[0126] S3, the oil phase material after the dechlorination reaction enters the dehydrogenation-neutralization reactor 14, where hydrogen (Si-H) is removed under the action of a catalyst, and at the same time, it undergoes a neutralization reaction with alkaline water;
[0127] S4, the oil phase material after the dehydrogenation-neutralization reaction enters the polymerization reactor 18 and undergoes polymerization under the action of solid acid molecular sieve;
[0128] S5, after the polymerization reaction, the oil phase material is subjected to vacuum de-lowering treatment to remove low-component substances, resulting in an inert high-boiling silicone oil product.
[0129] Furthermore, in step S1, the high-boiling substance is an organosilicon high-boiling substance.
[0130] Furthermore, in step S1, concentrated hydrochloric acid and high-boiling substances first enter the pre-reactor 4, where they are mixed and pre-reacted before entering the reaction tower 1 for hydrolysis.
[0131] Furthermore, in step S1, the mass concentration of concentrated hydrochloric acid is 25-30%.
[0132] Furthermore, in step S1, the concentrated hydrochloric acid and high-boiling-point substances are added as follows: First, concentrated hydrochloric acid is added to the lower chamber 102 of the reaction tower 1, with the amount of concentrated hydrochloric acid added being slightly lower than the oil phase outlet of the reaction tower 1; then, the circulating pump 2 is turned on, and the concentrated hydrochloric acid is cooled by the heat exchanger 3 and pumped into the pre-reactor 4. The concentrated hydrochloric acid enters from the inlet of the venturi tube 401, while the high-boiling-point substances are drawn in from the throat on the side of the venturi tube 401, so that the concentrated hydrochloric acid and high-boiling-point substances are rapidly mixed in the venturi tube 401, and then further mixed and pre-reacted under the action of the material mixing structure 402.
[0133] As some embodiments of this application, in step S1, the amount of concentrated hydrochloric acid added is preferably 5 to 30 cm above the oil phase outlet of the reaction tower 1.
[0134] In some other embodiments of this application, in step S1, the size of the aqueous phase outlet of the reactor 1 can be controlled so that the residence time of concentrated hydrochloric acid in the reactor 1 is 1 to 3 hours.
[0135] Preferably, the flow ratio of concentrated hydrochloric acid to high-boiling-point substance is 50-100:1. That is, the flow ratio of circulating pump 2 to high-boiling-point substance is 50-100:1.
[0136] Furthermore, in step S1, the state of the heat exchanger 3 is adjusted so that the temperature of the material discharged from the pre-reactor 4 is 40-60°C.
[0137] Specifically, the material discharged from the pre-reactor 4 enters the feed port of the reaction tower 1, and then disperses and flows in the upper swirl structure 101 of the reaction tower 1 before entering the lower chamber 102 of the reaction tower 1. The hydrogen chloride gas generated by the reaction is discharged from the top of the reaction tower 1 and recycled. After the material enters the lower chamber 102 of the reaction tower 1, the oil and water separate, and the oil layer material flows into the first intermediate tank 5 from the oil phase outlet 103.
[0138] Furthermore, in step S1, the residence time of the oil phase in the reaction tower 1 can be 1 to 3 hours by adjusting the feed rate of the high-boiling-point substance, the size of the lower chamber 102 of the reaction tower 1, the level of concentrated hydrochloric acid and the height of the oil phase outlet 103; at the same time, the lower chamber 102 is replenished with water in a timely manner by monitoring the level of the interface liquid level gauge on the lower chamber 102 to control the amount of concentrated hydrochloric acid in the reaction tower 1.
[0139] Furthermore, after the oil layer material flows into the first intermediate tank 5 from the oil phase outlet 103, it can stay in the first intermediate tank 5 for 1 to 2 hours for further oil-water separation. The oil phase after oil-water separation overflows from the top of the first intermediate tank 5 and is then pumped into the dechlorination reactor 7; the water phase flows out from the bottom of the first intermediate tank 5 and returns, mixes with the water phase discharged from the reaction tower 1, and then re-enters the reaction tower 1 through the circulation pump 2.
[0140] Furthermore, the water phase level in the first intermediate tank 5 can be controlled between 0% and 20% of the total liquid level using an interface gauge on the first intermediate tank 5.
[0141] Furthermore, in step S2, the oil phase enters the dechlorination reactor from the top of the lower section 703, and the activated clay enters the dechlorination reactor 7 from below the first filter structure at the bottom of the upper section 701. At the same time, the temperature of the middle section 702 of the dechlorination reactor is controlled to be 70-100°C by the heating structure of the middle section 702, so that the oil phase removes unhydrolyzed chlorine (Si-Cl) in the middle section 702 of the dechlorination reactor under the action of high temperature and activated clay.
[0142] Furthermore, in step S2, the amount of activated clay used is 1 to 5% of the mass of the oil phase material in the dechlorination reactor 7.
[0143] Furthermore, in step S2, the residence time of the oil phase material in the middle section 702 of the dechlorination reactor is 2 to 4 hours.
[0144] Furthermore, in step S2, the activated clay and its byproducts such as HCl produced by adsorption and neutralization enter the lower section 703 of the dechlorination reactor. After settling, the filtrate enters the centrifuge 8 from the bottom of the dechlorination reactor 7 for filtration. The filtrate enters the second intermediate tank 9 and is then pumped back to the dechlorination reactor 7 for reuse by the second transfer pump 10.
[0145] Furthermore, in step S3, the oil phase material flows from the oil phase discharge port near the top of the dechlorination reactor 7 into the third intermediate tank 11, and then is pumped by the third transfer pump 13 from the top of the lower section 1403 of the dehydrogenation-neutralization reactor into the dehydrogenation-neutralization reactor 14. Then, in the middle section 1402 of the dehydrogenation-neutralization reactor, hydrogen (Si-H) is removed under the action of nickel chloride catalyst loaded on the packing, alkaline water and high temperature.
[0146] Furthermore, the alkaline solution is one or more of sodium carbonate solution, sodium bicarbonate solution, or ammonia solution.
[0147] Furthermore, the alkaline water enters the dehydrogenation-neutralization reactor from the bottom of the upper section 1401 of the dehydrogenation-neutralization reactor to neutralize the oil phase inside.
[0148] Preferably, the amount of alkaline solution used is determined according to the acid value in the oil phase, and the amount of alkaline solution used is 2 to 4 times the calculated molar number of HCl.
[0149] Furthermore, in step S3, the middle section 1402 of the dehydrogenation-neutralization reactor is equipped with a heating structure, which maintains its temperature at 80-100°C.
[0150] Furthermore, in step S3, the residence time of the oil phase and aqueous phase materials in the middle section 1402 of the dehydrogenation-neutralization reactor is 2 to 4 hours.
[0151] Furthermore, in step S4, the oil phase flows from the outlet of the dehydrogenation-neutralization reactor at the top of the dehydrogenation-neutralization reactor 14 into the fifth intermediate tank 16, and then is sent to the bottom of the polymerization reactor 18 by the fourth transfer pump 17, where the polymerization reaction takes place under the action of the solid acid molecular sieve in the polymerization reactor 18.
[0152] Preferably, the residence time of the oil phase material in the heating section of the polymer reactor 18 is 1 to 2 hours.
[0153] Furthermore, in step S5, the oil phase material after the polymerization reaction is discharged from the outlet of the polymerization reactor 18 to the sixth intermediate tank 19, and then sent to the thin film evaporator 21 by the fifth transfer pump 20 for vacuum de-lowering treatment. After removing low-component substances, inert high-boiling silicone oil product is obtained. The removed low-component substances are condensed and enter the seventh intermediate tank 23, and then sent to the polymerization reactor 18 for reuse by the sixth transfer pump 22.
[0154] Preferably, in step S5, the outlet temperature of the thin-film evaporator 21 is controlled to be 100-160°C.
[0155] The following specific embodiments illustrate the inert high-boiling silicone oil production line and its production process according to the present invention:
[0156] Example 1
[0157] 25% concentrated hydrochloric acid is added to the lower chamber 102 of the reaction tower. The level of the concentrated hydrochloric acid is 5 cm below the oil phase outlet of the reaction tower. Then, the circulation pump is turned on, and the concentrated hydrochloric acid is cooled by the heat exchanger and pumped into the pre-reactor. The concentrated hydrochloric acid enters from the inlet of the venturi tube, while the high-boiling-point substance is drawn in from the throat on the side of the venturi tube, so that the concentrated hydrochloric acid and the high-boiling-point substance are rapidly mixed in the venturi tube. Then, under the action of the material mixing structure, they are further mixed and pre-reacted. The flow ratio of concentrated hydrochloric acid to high-boiling-point substance is 50:1. At the same time, the state of the heat exchanger is controlled so that the temperature of the material discharged from the pre-reactor is 41℃.
[0158] The material discharged from the pre-reactor enters the reaction tower through the feed inlet, then disperses and flows within the swirl structure at the top of the reaction tower before entering the lower chamber. The oil phase remains in the reaction tower for 1 hour, and the hydrogen chloride gas produced by the reaction is discharged from the top of the reaction tower for recycling. After entering the lower chamber of the reaction tower, the oil and water separate. The oil layer flows into the first intermediate tank from the oil phase outlet and remains there for 1 hour for further oil-water separation. The oil phase after oil-water separation overflows from the top of the first intermediate tank and is then pumped into the dechlorination reactor. The water phase flows out from the bottom of the first intermediate tank and returns, mixing with the water phase discharged from the reaction tower before being pumped back into the reaction tower.
[0159] The oil phase enters the dechlorination reactor from the top of the lower section, while the activated clay enters from below the first filter structure at the bottom of the upper section. The amount of activated clay used is 1% of the oil phase mass. Simultaneously, the temperature in the middle section of the dechlorination reactor is controlled at 70-80℃ by the heating structure, allowing the oil phase to remove unhydrolyzed chlorine (Si-Cl) under the influence of high temperature and activated clay. The residence time of the oil phase in the middle section of the dechlorination reactor is 2 hours. The activated clay and its adsorption and neutralization byproducts, such as HCl, enter the lower section of the dechlorination reactor. After sedimentation, the filtrate enters a centrifuge at the bottom of the dechlorination reactor for filtration. The filtrate enters the second intermediate tank and is then pumped back to the dechlorination reactor for reuse via a second transfer pump. The oil phase material flows from the oil phase discharge port near the top of the dechlorination reactor into the third intermediate tank, and is then pumped from the top of the lower section of the dehydrogenation-neutralization reactor into the dehydrogenation-neutralization reactor via a third transfer pump.
[0160] In the middle section of the dehydrogenation-neutralization reactor, hydrogen (Si-H) is removed under the action of nickel chloride catalyst supported on the packing material, alkaline water, and high temperature; wherein, the alkaline water is a sodium carbonate solution, and the amount of alkaline water is twice the calculated molar number of HCl; the temperature in the middle section of the dehydrogenation-neutralization reactor is maintained at 80-85℃; the residence time of oil phase and water phase materials in the middle section of the dehydrogenation-neutralization reactor is 2 hours;
[0161] Afterwards, the oil phase flows from the dehydrogenation-neutralization reaction outlet at the top of the dehydrogenation-neutralization reactor into the fifth intermediate tank, and then is sent to the bottom of the polymerization reactor by the fourth transfer pump. The polymerization reaction is carried out in the polymerization reactor under the action of solid acid molecular sieve. The residence time of the oil phase material in the heating section of the polymerization reactor is 1 hour.
[0162] After the polymerization reaction, the oil phase material is discharged from the discharge port of the polymerization reactor to the sixth intermediate tank, and then sent to the thin film evaporator by the fifth transfer pump for vacuum de-lowering treatment. The outlet temperature of the thin film evaporator is controlled at 100℃. After removing the low-component substances, inert high-boiling silicone oil is obtained. The removed low-component substances are condensed and enter the seventh intermediate tank, and then sent to the polymerization reactor for reuse by the sixth transfer pump.
[0163] The inert high-boiling silicone oil product obtained in Example 1 was tested and the following results were obtained: Kinematic viscosity (25°C) of the inert high-boiling silicone oil product: 340 mmHg 2 / s; Chloride ion content: 2.3ppm; Volatile matter: 1.3%; Hydrogen: Not detected; Color / Hazen units (Platinum-Cobalt color number): 20.
[0164] In summary, the inert high-boiling silicone oil production line and its production process described in this invention have the following advantages:
[0165] First, the production line and production process of the inert high-boiling silicone oil described in this invention provide a continuous production technology for preparing high-boiling silicone oil using organosilicon high-boiling substances. The production and preparation process of high-boiling silicone oil is simple, controllable, and suitable for industrial continuous production, and can obtain high-quality high-boiling silicone oil with low chloride ion content, no hydrogen content, and controllable viscosity.
[0166] Secondly, the high-boiling silicone oil prepared by this invention does not contain active groups and is an inert high-boiling silicone oil, which can be used in the production of organosilicon coatings, silicone rubber, etc.
[0167] Third, the production line and process of the inert high-boiling silicone oil described in this invention use concentrated hydrochloric acid and high-boiling substances for hydrolysis reaction, which is conducive to uniform reaction; at the same time, the use of a high-flow-rate circulating pump to circulate and cool the concentrated hydrochloric acid before mixing it with the high-boiling substances for reaction is conducive to timely absorption of the heat generated by the reaction; at the same time, it can make the reaction temperature uniform and stable, which is conducive to temperature control; in addition, by mixing the high-boiling substances with a high-flow-rate concentrated hydrochloric acid, it is beneficial for the high-boiling substances to react quickly and fully.
[0168] Fourth, by setting a swirling structure at the top of the reaction tower, the material can flow from the top of the reaction tower to the bottom of the tower in a swirling manner, which is beneficial to the dispersion of the material, and at the same time, it is beneficial to the timely discharge of hydrogen chloride produced by the reaction and to promote the mixing and reaction of the material.
[0169] Fifth, activated clay is used for dechlorination. The activated clay can remove Cl from the difficult-to-hydrolyze Si-Cl at higher temperatures. At the same time, activated clay has the functions of decolorization, adsorption of hydrogen chloride, and adsorption of impurities. In addition, after dechlorination, the oil phase can be neutralized with a small amount of low-concentration alkaline water in the dehydrogenation-neutralization stage to obtain high-boiling silicone oil with low chloride ion (low acid value), saving the amount of alkali used.
[0170] Sixth, the packing material in the middle section of the dehydrogenation-neutralization reactor is made by adsorbing nickel chloride solution and sintering, which has the function of rapidly removing H from Si-H in the oil phase, so that the prepared inert high-boiling silicone oil is basically free of Si-H.
[0171] Seventh, the alkaline solution used during dehydrogenation-neutralization is a weak alkaline solution such as ammonia water, sodium carbonate solution, or sodium bicarbonate solution. Strong alkaline solutions should not be used to avoid the formation of silicone oil gel.
[0172] Eighth, in the polymerization reaction, solid acid molecular sieves are used, which result in a fast reaction and a long service life, instead of the conventionally used liquid alkali and liquid acid. This avoids the disadvantages of liquid alkali and liquid acid having a rapid decrease in concentration after use and a low number of uses, and reduces the discharge of waste acid and waste alkali.
[0173] The embodiments of this application have been described above with reference to the accompanying drawings. Unless otherwise specified, the embodiments and features in the embodiments of this application can be combined with each other. This application is not limited to the specific embodiments described above. The specific embodiments described above are merely illustrative and not restrictive. Those skilled in the art can make many other forms under the guidance of this application without departing from the spirit and scope of the claims, and all of these forms are within the protection scope of this application.
Claims
1. A production line for inert high-boiling silicone oil, characterized in that, Including the following settings in sequence: A hydrolysis reaction unit includes a reaction tower (1), into which concentrated hydrochloric acid and high-boiling substances are introduced to carry out a hydrolysis reaction; The dechlorination reaction unit includes a dechlorination reactor (7), in which oil phase substances discharged from the reaction tower (1) enter the dechlorination reactor (7) and undergo a dechlorination reaction with activated clay to remove unhydrolyzed chlorine; The dehydrogenation-neutralization reaction unit includes a dehydrogenation-neutralization reactor (14), which includes an upper section (1401), a middle section (1402), and a lower section (1403). The middle section (1402) of the dehydrogenation-neutralization reactor is equipped with sintered nickel chloride adsorbent packing. The oil phase material discharged from the dechlorination reactor (7) enters the dehydrogenation-neutralization reactor (14) to carry out dehydrogenation and neutralization reactions. The polymerization reaction unit includes a polymerization reactor (18) into which oil phase substances discharged from the dehydrogenation-neutralization reactor (14) enter the polymerization reactor (18) for polymerization reaction; The oil phase material discharged from the polymerization reactor (18) enters the evaporation unit, and after evaporation to remove low-component materials, an inert high-boiling silicone oil product is obtained.
2. The production line for inert high-boiling silicone oil according to claim 1, characterized in that, The hydrolysis reaction unit further includes: The pre-reactor (4) has its feed end connected to the water phase outlet of the bottom of the reaction tower (1) and its outlet end connected to the feed inlet at the top of the reaction tower (1). Concentrated hydrochloric acid and high-boiling substances are first mixed in the pre-reactor (4) and pre-reacted, and then enter the reaction tower (1) to undergo a full hydrolysis reaction. The pre-reactor (4) includes a pre-reactor front section and a pre-reactor rear section: A venturi tube (401) is installed at the front end of the pre-reactor. Hydrochloric acid enters the pre-reactor (4) from the inlet of the venturi tube (401). At the same time, a negative pressure is generated at the throat of the venturi tube (401). Under the action of this negative pressure, high-boiling substances are drawn into the venturi tube (401). A material mixing structure (402) is provided in the rear section of the pre-reactor. The material mixing structure (402) includes multiple baffles that are staggered in the rear section of the pre-reactor, and the baffles form a serpentine material channel in the rear section of the pre-reactor.
3. The production line for inert high-boiling silicone oil according to claim 1, characterized in that, The reaction tower (1) is divided into an upper section and a lower section. A swirling structure (101) is provided in the upper section and a lower cavity (102) is formed in the lower section.
4. The production line for inert high-boiling silicone oil according to claim 1, characterized in that, The dechlorination reactor (7) includes: an upper section (701), a middle section (702), and a lower section (703). A first filter structure is provided in the upper section (701) of the dechlorination reactor, and the first filter structure is located in the lower part of the upper section (701) of the dechlorination reactor; A heating structure is provided in the middle section (702) of the dechlorination reactor; The lower section (703) of the dechlorination reactor is provided with a feed inlet at the top and a by-product discharge outlet at the bottom.
5. The production line for inert high-boiling silicone oil according to claim 1, characterized in that: A heating structure is provided in the middle section (1402) of the dehydrogenation-neutralization reactor; The sum of the volumes of the upper section (1401) and the lower section (1403) of the dehydrogenation-neutralization reactor is 30 to 50% of the volume of the middle section (1402) of the dehydrogenation-neutralization reactor.
6. The production line for inert high-boiling silicone oil according to claim 1, characterized in that, The top of the tunable polymerization reactor (18) is an vent, the side near the top is provided with a discharge port, and the bottom is provided with a feed port. The top and bottom of the tunable polymerization reactor (18) are respectively provided with a second filter structure, and a heating structure is provided in the second filter structure to maintain the temperature of the second filter structure at 80~100℃.
7. The production line for inert high-boiling silicone oil according to claim 1, characterized in that, The evaporation unit includes: In the thin film evaporator (21), the oil phase material discharged from the polymer reactor (18) to the thin film evaporator (21) undergoes vacuum de-lowering treatment to remove low-component substances.
8. The production line for inert high-boiling silicone oil according to claim 7, characterized in that, The evaporation unit further includes: The seventh intermediate tank (23) is connected to the low component material outlet on the thin film evaporator (21). The low component material removed by vacuum de-lowering treatment is condensed and stored in the seventh intermediate tank (23). The sixth transfer pump (22) is connected to the seventh intermediate tank (23) and the chelation reactor (18) respectively, and is used to transport and reuse the material in the seventh intermediate tank (23) to the chelation reactor (18).
9. A production process for an inert high-boiling-point silicone oil, characterized in that, The production process uses the production line described in any one of claims 1 to 8 to prepare inert high-boiling silicone oil, and the production process includes the following steps: S1, concentrated hydrochloric acid and high-boiling substances undergo hydrolysis reaction in the reaction tower; S2, the oil phase material after hydrolysis reaction reacts with activated clay in the dechlorination reactor to remove the unhydrolyzed chlorine; S3, the oil phase material after the dechlorination reaction enters the dehydrogenation-neutralization reactor, where hydrogen is removed under the action of a catalyst, and at the same time, it undergoes a neutralization reaction with alkaline water; S4, the oil phase material after the dehydrogenation-neutralization reaction enters the polymerization reactor and undergoes polymerization under the action of solid acid molecular sieve; S5, after the polymerization reaction, the oil phase material is subjected to vacuum de-lowering treatment to remove low-component substances, resulting in an inert high-boiling silicone oil product.
10. The production process of the inert high-boiling silicone oil according to claim 9, characterized in that, In step S1, the mass concentration of concentrated hydrochloric acid is 25-30%; the flow ratio of concentrated hydrochloric acid to high-boiling-point substance is 50-100:1; the residence time of the oil phase substance in the reaction tower is controlled to be 1-3 hours; the method of adding concentrated hydrochloric acid and high-boiling-point substance is as follows: first, concentrated hydrochloric acid is added to the lower chamber of the reaction tower, and the liquid level of concentrated hydrochloric acid is controlled to be lower than the oil phase outlet of the reaction tower. Then, the circulation pump is turned on, and the concentrated hydrochloric acid is cooled by the heat exchanger and pumped into the pre-reactor. The concentrated hydrochloric acid enters from the inlet of the venturi tube, and at the same time, the high-boiling-point substance is drawn in from the throat on the side of the venturi tube. In step S2, the amount of activated clay used is 1-5% of the mass of the oil phase material; the temperature in the middle section of the dechlorination reactor is 70-100℃, and the residence time of the oil phase material in the middle section of the dechlorination reactor is 2-4 hours. In step S3, the alkaline solution is one or more of sodium carbonate solution, sodium bicarbonate solution, or ammonia solution, the temperature in the middle section of the dehydrogenation-neutralization reactor is maintained at 80-100℃, and the residence time of the material in the middle section of the dehydrogenation-neutralization reactor is 2-4 hours. In step S4, the residence time of the oil phase material in the heating section of the polymer reactor is 1 to 2 hours.
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