MQ silicon resin suitable for leather manufacturing and industrial control method

Abstract

The invention discloses an MQ silicon resin suitable for leather manufacturing and an industrial control method, and belongs to the technical field of MQ silicon resin production, water glass and pure water are adopted as raw materials, a hydrolysis reaction is performed in a reaction kettle under the action of an acid catalyst, then an end-capping reagent and a solvent are added for an end-capping reaction, and the MQ silicon resin is obtained. After standing for oil-water separation, a first oil phase flows into a first mixer, an acid catalyst is added into the first mixer for acid pickling, after acid pickling is completed, first oil-water separation is conducted, a second oil phase flows into a second mixer, and a salt washing reagent is added into the second mixer for salt washing; after salt washing is completed, second oil-liquid separation is conducted, then a third oil phase flows into a third mixer, an alkali washing reagent is added into the third mixer for alkali washing, third oil-liquid separation is conducted after alkali washing is completed, then a fourth oil phase flows into a fourth mixer, desalted water is added into the fourth mixer for water washing, and third oil-liquid separation is conducted; and after the water washing is finished, carrying out fourth oil-liquid separation, and enabling a fifth oil phase to flow into the drying kettle for drying treatment.

Description

Technical Field

[0001] The invention relates to the technical field of MQ silicone resin production, and in particular to an MQ silicone resin suitable for leather manufacturing and an industrial control method. Background Art

[0002] Leather materials have been widely used in many fields such as automobiles, aviation, medical treatment, clothing, luggage, furniture, decoration, etc. due to their good physical and mechanical properties, excellent hygiene properties, and exquisite appearance and texture. They are closely related to people's daily life, work, travel and other aspects, and have become indispensable materials. According to the source of the material, leather materials are generally divided into two categories: natural leather and artificial leather. According to data from relevant websites, my country's annual production and sales of natural leather are about 500 million square meters, accounting for about 20% of the global total, and the annual production and sales of artificial leather are about 4 billion square meters, accounting for about 60% of the global total, and the market space is huge. However, the leather industry is currently facing development bottlenecks in environmental protection and product performance, and cannot meet the requirements of the country's green environmental protection policies and people's demand for high-performance leather.

[0003] Silicone synthetic leather is a new type of artificial leather that has emerged in recent years. It uses liquid silicone rubber (LSR) as the main raw material and adopts the curing method of silicon hydrogen addition. There is no small molecule release during the production process, which is in line with my country's concept of green development. Due to the unique -Si-O-Si-main chain of polysiloxane and the outward spiral structure of methyl, silicone leather has the characteristics of weather resistance, anti-fouling, skin-friendly, high and low temperature resistance, flame retardant, chemical corrosion resistance, and breathability. However, silicone leather production requires LSR, which has a lower viscosity, while solvent-free LSR is difficult to meet both low viscosity and high strength. In addition, LSR has low surface energy and lacks active groups that react with the base fabric. Therefore, silicone leather has problems such as poor processing performance, strength, wear resistance, and interlayer bonding performance.

[0004] A Chinese patent with publication number CN114058276A and publication date 2022-02-18 discloses a solvent-free, high folding resistance, high wear-resistant silicone leather and a preparation method thereof. The methacryloyloxy MQ resin has a vinyl content of 2wt%-3wt% and a structural formula as shown in formula (1): Formula (1); Among them, R 1 for ; n=an integer of 1-10; R 2It can be methyl, ethyl, propyl, phenyl, or hydroxyl; the methacryloxy MQ resin is prepared by the following steps: (1) adding tetraethoxysilane to a reaction bottle, dripping HCl solution, performing hydrolysis polymerization reaction under acid catalysis, adding hexamethyldisiloxane and bis-3-methacryloxypropylated tetramethyldisiloxane, methacryloxypropyltrimethoxysilane or other silane monomers containing methacryloxy groups, continuing hydrolysis polymerization reaction, adding isoparaffin extraction after the reaction is completed, standing and separating the liquids to obtain an upper prepolymer solution; (2) adding the upper prepolymer solution to a reaction bottle, adding KOH methanol solution, performing alkaline condensation reaction, adding NaHCO3, neutralizing and filtering to obtain a methacryloxy MQ resin solution, and then distilling and drying under reduced pressure to obtain a methacryloxy MQ resin. The preparation method of the methacryloxy MQ resin for silicone leather cannot be automatically controlled, and the production cost is relatively high. Summary of the invention

[0005] The present invention aims to solve the problems existing in the prior art and provides an MQ silicone resin and an industrial control method suitable for leather manufacturing. The invention has high production efficiency and adopts an uninterrupted production method. The equipment can operate stably for a long time and has a high output per unit time. This also makes the product quality stable and high, with a high degree of automation, reducing human intervention and environmental impact, which not only improves production efficiency, but also reduces quality problems and safety hazards caused by human errors.

[0006] The objective of the present invention is achieved through the following technical solutions: A MQ silicone resin suitable for leather manufacturing, with the general formula (Me 3 SiO 1 / 2 )a(Me 2 ViSiO 3 / 2 )b(SiO 4 / 2 )c; Having the structural formula: Among them: weight average molecular weight 4000~5500 Da; Molecular weight distribution 1.3~2.0; The viscosity of xylene with 60% solid content is 5~15cst; The hydroxyl content is 0.5~2%; M / Q is 0.9~1.0; Vinyl content is 2.0~3.0%; Light transmittance: 99%~100%; Acid value: 0~20ppm.

[0007] Preferably, in the general formula, a=15-30; b=3-10; c=20-30.

[0008] An industrial control method for MQ silicone resin suitable for leather manufacturing, using water glass and pure water as raw materials, hydrolyzing reaction in a reactor under the action of an acid catalyst, then adding a capping agent and a solvent for capping reaction, standing for oil-water separation, flowing a first oil phase into a first mixer, adding an acid catalyst to the first mixer for pickling, after the pickling is completed, performing a first oil-liquid separation, flowing a second oil phase into a second mixer, adding a salt washing agent to the second mixer for salt washing, after the salt washing is completed, performing a second oil-liquid separation, flowing a third oil phase into a third mixer, adding an alkali washing agent to the third mixer for alkali washing, after the alkali washing is completed, performing a third oil-liquid separation, flowing a fourth oil phase into a fourth mixer, adding desalted water to the fourth mixer for water washing, after the water washing is completed, performing a fourth oil-liquid separation, flowing a fifth oil phase into a drying kettle for drying treatment; During the reaction process, at least the following control methods are included: (I) The DCS interlock controller controls the temperature of the acid catalyst storage tank, solvent storage tank, water glass solution storage tank and end-capping agent storage tank; (II) The DCS linkage controller controls the opening and closing of the acid catalyst diaphragm pump, the opening and closing of the water glass solution diaphragm pump, the opening and closing of the end-capping agent diaphragm pump, the opening and closing of the acid catalyst feed valve, the opening and closing of the water glass solution feed valve, the opening and closing of the end-capping agent feed valve, the opening and closing of the solvent feed valve and the opening and closing of the reactor discharge valve; (III) The DCS linkage controller controls the opening and closing of the reactor stirring device, the speed of the reactor stirring device, the time of the end-capping reaction and the temperature of the reactor heat exchange jacket; (IV) The DCS linkage controller controls the temperature of the first mixer, the flow rate of the oil phase flowing into the first mixer, the flow rate of the acid catalyst flowing into the first mixer, and the opening and closing of the discharge valve of the first mixer; (V), the DCS linkage controller controls the temperature of the second mixer, the flow rate of the first oil phase into the second mixer, the flow rate of the salt washing reagent into the second mixer, and the opening and closing of the discharge valve of the second mixer; (VI), a DCS linkage controller controls the temperature of the third mixer, the flow rate of the second oil phase flowing into the third mixer, the flow rate of the alkali washing agent flowing into the third mixer, and the opening and closing of the discharge valve of the third mixer; (VII), the DCS linkage controller controls the temperature of the fourth mixer, the flow rate of the third oil phase flowing into the fourth mixer, the flow rate of the water washing reagent flowing into the fourth mixer, and the opening and closing of the discharge valve of the fourth mixer; (VIII) The DCS linkage controller controls the temperature, drying time, vacuum degree and stirring speed in the drying kettle.

[0009] Preferably, the DCS linkage controller controls the temperature of the acid catalyst storage tank, the solvent storage tank, the water glass solution storage tank and the end-capping agent storage tank at 5-25°C. When the storage tank temperature is lower than 7°C, the DCS control system controls the storage tank heat exchange jacket to start hot water circulation; when the storage tank temperature is higher than 23°C, the DCS control system controls the storage tank heat exchange jacket to start cold water circulation; the density of the water glass solution is 1.0-1.5 g / cm 3 , modulus is 3.0~3.6, silicon dioxide content is 7~10%; the acid catalyst is selected from one of concentrated sulfuric acid, hydrochloric acid, phosphoric acid, and p-toluenesulfonic acid, wherein water: water glass solution: catalyst = 4:2~3:2; the end-capping agent is a methyl end-capping agent and a vinyl end-capping agent, the methyl end-capping agent is selected from any one of trimethylchlorosilane or hexamethyldisiloxane, and the vinyl end-capping agent is selected from any one of dimethylvinylethoxysilane or 1,3-divinyltetramethyldisiloxane; the solvent is selected from any one of isopropanol or ethanol, and the end-capping agent: solvent = 1:4~6.

[0010] Preferably, the acid catalyst feed valve is opened first, and the acid catalyst feed valve is closed 30 seconds after the acid catalyst is added; the reactor stirring device is opened after 2 to 5 minutes, and the speed of the reactor stirring device is 200 to 300 r / min; the water glass solution feed valve is opened, and the water glass solution feed valve is closed 30 seconds after the water glass solution is added, and the hydrolysis reaction time of the water glass solution under the action of the acid catalyst is 0 to 80 seconds; then the end-capping agent feed valve is opened, and the end-capping agent feed valve is closed 30 seconds after the end-capping agent is added; the temperature of the reactor heat exchange jacket is controlled to 30 to 60°C, the reactor heat exchange jacket is stopped after 0.5 to 2.0 hours, and the reactor stirring device is closed after reacting for 2 to 3 hours.

[0011] Preferably, after standing for 30 minutes, the reactor wastewater discharge valve is fully opened and the medium density is between 0.8 and 0.85 g / cm 3 Then close the reactor wastewater discharge valve, let it stand for 10-30 minutes, and adjust the opening of the reactor wastewater discharge valve to 25-50% again. The medium density is between 0.8-0.85 g / cm 3 Then close the reactor wastewater discharge valve, let it stand for 10-30 minutes, and adjust the opening of the reactor wastewater discharge valve to 25-50% again. Repeat the above steps 3 times until the density data stabilizes at 0.8-0.85 g / cm 3 Then close the reactor wastewater discharge valve; then open the first mixer discharge valve.

[0012] Preferably, the temperature of the first mixer is controlled at 10-50°C, the flow rate of the oil phase flowing into the first mixer is 30-60 g / s, and the flow rate of the acid catalyst flowing into the first mixer is 5-10 g / s; after the oleic acid mixture passes through the first mixer, the discharge valve at the lower end of the first mixer is opened, and the material is transferred to the first stratification tank for standing for oil-water separation, and the temperature of the first stratification tank is controlled at 10-40°C. When the liquid level of the first stratification tank reaches 25-30%, the upper discharge valve of the first stratification tank is opened, and the opening of the upper discharge valve of the first stratification tank is controlled so that the flow rate of the first oil phase is 30-60 g / s; the lower discharge valve of the first stratification tank is opened, and the opening of the lower discharge valve of the first stratification tank is controlled so that the flow rate of the wastewater in the first stratification tank is 5-10 g / s.

[0013] Preferably, the temperature of the second mixer is controlled at 20-80°C, the flow rate of the first oil phase in the first stratification tank flowing into the second mixer is 30-60 g / s, and the flow rate of the salt washing reagent flowing into the second mixer is 5-20 g / s; after the oil-water mixture passes through the second mixer, the discharge valve at the lower end of the second mixer is opened to transfer the material to the second stratification tank for standing to separate oil and water, and the temperature of the second stratification tank is controlled at 20-60°C. When the liquid level of the second stratification tank reaches 30-35%, the upper discharge valve of the second stratification tank is opened, and the opening of the upper discharge valve of the second stratification tank is controlled so that the flow rate of the second oil phase is 30-60 g / s; the lower discharge valve of the second stratification tank is opened, and the opening of the lower discharge valve of the second stratification tank is controlled so that the flow rate of the waste water in the second stratification tank is 5-20 g / s.

[0014] Preferably, the temperature of the third mixer is controlled at 20-70°C, the flow rate of the second oil phase in the second stratification tank flowing into the third mixer is 30-60 g / s, and the flow rate of the alkali washing agent flowing into the third mixer is 10-30 g / s; after the oil-water mixture passes through the third mixer, the discharge valve at the lower end of the third mixer is opened, and the material is transferred to the third stratification tank for standing for oil-water separation, and the temperature of the third stratification tank is controlled at 20-60°C. When the liquid level of the third stratification tank reaches 30-35%, the upper discharge valve of the third stratification tank is opened, and the opening of the upper discharge valve of the third stratification tank is controlled so that the flow rate of the third oil phase is 30-60 g / s; the lower discharge valve of the third stratification tank is opened, and the opening of the lower discharge valve of the third stratification tank is controlled so that the flow rate of the waste water in the third stratification tank is 10-30 g / s.

[0015] Preferably, the temperature of the fourth mixer is controlled to be 20-80°C, the flow rate of the third oil phase in the third stratification tank flowing into the fourth mixer is 30-60 g / s, and the flow rate of desalted water flowing into the fourth mixer is 10-30 g / s; after the oil-water mixture passes through the third mixer, the discharge valve at the lower end of the fourth mixer is opened, and the material is transferred to the fourth stratification tank for standing for oil-water separation, and the temperature of the fourth stratification tank is controlled at 20-50°C. When the liquid level of the fourth stratification tank reaches 30-35%, the upper discharge valve of the fourth stratification tank is opened, and the opening of the upper discharge valve of the fourth stratification tank is controlled so that the flow rate of the fourth oil phase is 30-60 g / s; the lower discharge valve of the fourth stratification tank is opened, and the opening of the lower discharge valve of the fourth stratification tank is controlled so that the flow rate of the waste water in the fourth stratification tank is 10-30 g / s.

[0016] Preferably, the temperature in the drying kettle is 80-180° C., the drying time is 1-3 h, the vacuum degree is 0.08-0.1 MPa, and the stirring speed is 10-50 rpm.

[0017] The beneficial effects of this technical solution are as follows: 1. The present invention provides an MQ silicone resin suitable for leather manufacturing. By controlling the formation of M-Q bonds and Q-Q bonds (i.e., the competitive reaction between end-capping condensation and sol condensation), an MQ silicone resin with a high M / Q ratio (0.9-1.0), a specific vinyl content (2.0-3.0%), and a molecular weight (Mw=4000-5500) structure is prepared. The resin can not only make the silicone leather have high strength, high toughness and resilience, but also improve weather resistance, oil and water resistance. At the same time, due to the long Si-O-Si bond length and large bond angle, the multi-branched 3D structure of the MQ silicone resin can increase the cross-linking sites with the raw rubber, but will not increase the hardness, so that the silicone leather has good air permeability and wear resistance.

[0018] 2. The MQ silicone resin suitable for leather manufacturing provided by the present invention is prepared by a solvent-free method, is green, environmentally friendly and sustainable throughout its life cycle, has excellent biocompatibility and low volatility, is an environmentally friendly green product, and can be used in vehicle interiors, home leather goods and other fields.

[0019] 3. The present invention provides an industrial control method for MQ silicone resin suitable for leather manufacturing, and establishes an automated system for large-scale production. The system can be applied to the production of MQ silicone resins of various structures. A continuous production method is adopted, and the output per unit time is high, which improves production efficiency, reduces manual intervention and environmental impact, makes product quality stable and high, and reduces safety hazards. The ability to accurately deliver raw materials and process control not only reduces the waste of raw materials, but also controls the production of defective products, thereby reducing production costs. At the same time, automated control reduces dependence on manual operations and reduces labor costs. DETAILED DESCRIPTION

[0020] The present invention is further described in detail below in conjunction with examples, but the embodiments of the present invention are not limited thereto.

[0021] Example 1 An industrial control method for MQ silicone resin suitable for leather manufacturing, using water glass and pure water as raw materials, hydrolyzing reaction in a reactor under the action of an acid catalyst, then adding a capping agent and a solvent for capping reaction, standing for oil-water separation, flowing a first oil phase into a first mixer, adding an acid catalyst to the first mixer for pickling, performing a first oil-liquid separation after pickling, flowing a second oil phase into a second mixer, adding a salt washing agent to the second mixer for salt washing, performing a second oil-liquid separation after salt washing, flowing a third oil phase into a third mixer, adding an alkali washing agent to the third mixer for alkali washing, performing a third oil-liquid separation after alkali washing, flowing a fourth oil phase into a fourth mixer, adding desalted water to the fourth mixer for water washing, performing a fourth oil-liquid separation after water washing, and flowing a fifth oil phase into a drying kettle for drying; During the reaction process, at least the following control methods are included: (I) The DCS interlock controller controls the temperature of the acid catalyst storage tank, solvent storage tank, water glass solution storage tank and end-capping agent storage tank; (II) The DCS linkage controller controls the opening and closing of the acid catalyst diaphragm pump, the opening and closing of the water glass solution diaphragm pump, the opening and closing of the end-capping agent diaphragm pump, the opening and closing of the acid catalyst feed valve, the opening and closing of the water glass solution feed valve, the opening and closing of the end-capping agent feed valve, the opening and closing of the solvent feed valve and the opening and closing of the reactor discharge valve; (III) The DCS linkage controller controls the opening and closing of the reactor stirring device, the speed of the reactor stirring device, the time of the end-capping reaction and the temperature of the reactor heat exchange jacket; (IV) The DCS linkage controller controls the temperature of the first mixer, the flow rate of the oil phase flowing into the first mixer, the flow rate of the acid catalyst flowing into the first mixer, and the opening and closing of the discharge valve of the first mixer; (V), the DCS linkage controller controls the temperature of the second mixer, the flow rate of the first oil phase into the second mixer, the flow rate of the salt washing reagent into the second mixer, and the opening and closing of the discharge valve of the second mixer; (VI), a DCS linkage controller controls the temperature of the third mixer, the flow rate of the second oil phase flowing into the third mixer, the flow rate of the alkali washing agent flowing into the third mixer, and the opening and closing of the discharge valve of the third mixer; (VII), the DCS linkage controller controls the temperature of the fourth mixer, the flow rate of the third oil phase flowing into the fourth mixer, the flow rate of the water washing reagent flowing into the fourth mixer, and the opening and closing of the discharge valve of the fourth mixer; (VIII) The DCS linkage controller controls the temperature, drying time, vacuum degree and stirring speed in the drying kettle.

[0022] The DCS linkage controller controls the temperature of the acid catalyst storage tank, solvent storage tank, water glass solution storage tank and end-capping agent storage tank at 6-10°C. When the storage tank temperature is lower than 7°C, the DCS control system controls the storage tank heat exchange jacket to start hot water circulation; when the storage tank temperature is higher than 9°C, the DCS control system controls the storage tank heat exchange jacket to start cold water circulation; the density of the water glass solution is 1.0g / cm 3 , modulus is 3.0, silicon dioxide content is 7%; the acid catalyst is concentrated sulfuric acid, wherein water: water glass solution: catalyst = 4:2:2; the end-capping agent is methyl end-capping agent and vinyl end-capping agent, the methyl end-capping agent is trimethylchlorosilane, and the vinyl end-capping agent is dimethylvinylethoxysilane; the solvent is isopropanol, and the end-capping agent: solvent = 1:4.

[0023] Among them, first open the acid catalyst feed valve, and close the acid catalyst feed valve 30s after the acid catalyst is added; open the reactor stirring device after 5min, and the speed of the reactor stirring device is 200r / min; open the water glass solution feed valve, and close the water glass solution feed valve 30s after the water glass solution is added, and the hydrolysis reaction time of the water glass solution under the action of the acid catalyst is 0s; then open the end-capping agent feed valve, and close the end-capping agent feed valve 30s after the end-capping agent is added; control the temperature of the reactor heat exchange jacket to 45°C, stop the reactor heat exchange jacket after 0.5h, and close the reactor stirring device after reacting for 2h.

[0024] After standing for 30 minutes, the reactor wastewater discharge valve was fully opened and the intelligent sight glass was used for detection. The medium density was 0.8 g / cm 3 Then close the reactor wastewater discharge valve, let it stand for 20 minutes, and adjust the opening of the reactor wastewater discharge valve to 25% again. The medium density is 0.8g / cm 3 Then close the reactor wastewater discharge valve, let it stand for 20 minutes, and adjust the opening of the reactor wastewater discharge valve to 25% again. Repeat the above steps 3 times until the density data stabilizes at 0.8~0.85g / cm 3 Then close the reactor wastewater discharge valve; then open the first mixer discharge valve.

[0025] Among them, the temperature of the first mixer is controlled to be 10°C, the flow rate of the oil phase flowing into the first mixer is 50g / s, and the flow rate of the acid catalyst flowing into the first mixer is 6g / s; after the oleic acid mixture passes through the first mixer, the discharge valve at the lower end of the first mixer is opened, and the material is transferred to the first stratification tank for standing for oil-water separation. The temperature of the first stratification tank is controlled at 10°C. When the liquid level of the first stratification tank reaches 25%, the upper discharge valve of the first stratification tank is opened, and the opening of the upper discharge valve of the first stratification tank is controlled so that the flow rate of the first oil phase is 50g / s; the lower discharge valve of the first stratification tank is opened, and the opening of the lower discharge valve of the first stratification tank is controlled so that the flow rate of the wastewater in the first stratification tank is 6g / s.

[0026] Among them, the temperature of the second mixer is controlled at 30°C, the flow rate of the first oil phase in the first stratification tank flowing into the second mixer is 50g / s, and the flow rate of the salt washing reagent flowing into the second mixer is 10g / s; after the oil-water mixture passes through the second mixer, the discharge valve at the lower end of the second mixer is opened to transfer the material to the second stratification tank for standing for oil-water separation, and the temperature of the second stratification tank is controlled at 25°C. When the liquid level of the second stratification tank reaches 30%, the upper discharge valve of the second stratification tank is opened, and the opening of the upper discharge valve of the second stratification tank is controlled so that the flow rate of the second oil phase is 50g / s; the lower discharge valve of the second stratification tank is opened, and the opening of the lower discharge valve of the second stratification tank is controlled so that the flow rate of the waste water in the second stratification tank is 10g / s.

[0027] Among them, the temperature of the third mixer is controlled at 30°C, the flow rate of the second oil phase in the second stratification tank flowing into the third mixer is 50g / s, and the flow rate of the alkaline washing agent flowing into the third mixer is 20g / s; after the oil-water mixture passes through the third mixer, the discharge valve at the lower end of the third mixer is opened, and the material is transferred to the third stratification tank for standing for oil-water separation. The temperature of the third stratification tank is controlled at 25°C. When the liquid level of the third stratification tank reaches 30%, the upper discharge valve of the third stratification tank is opened, and the opening of the upper discharge valve of the third stratification tank is controlled so that the flow rate of the third oil phase is 50g / s; the lower discharge valve of the third stratification tank is opened, and the opening of the lower discharge valve of the third stratification tank is controlled so that the flow rate of the waste water in the third stratification tank is 20g / s.

[0028] Among them, the temperature of the fourth mixer is controlled to be 30°C, the flow rate of the third oil phase in the third stratification tank flowing into the fourth mixer is 50g / s, and the flow rate of desalted water flowing into the fourth mixer is 20g / s; after the oil-water mixture passes through the third mixer, the discharge valve at the lower end of the fourth mixer is opened, and the material is transferred to the fourth stratification tank for standing for oil-water separation. The temperature of the fourth stratification tank is controlled at 25°C. When the liquid level of the fourth stratification tank reaches 30%, the upper discharge valve of the fourth stratification tank is opened, and the opening of the upper discharge valve of the fourth stratification tank is controlled so that the flow rate of the fourth oil phase is 50g / s; the lower discharge valve of the fourth stratification tank is opened, and the opening of the lower discharge valve of the fourth stratification tank is controlled so that the flow rate of the waste water in the fourth stratification tank is 20g / s.

[0029] The temperature in the drying kettle was 80°C, the drying time was 3h, the vacuum degree was 0.08MPa, and the stirring speed was 10rpm.

[0030] MQ silicone resin for leather manufacturing is obtained, with the general formula (Me 3 SiO 1 / 2 )a(Me 2 ViSiO 3 / 2 )b(SiO 4 / 2 )c; Among them: weight average molecular weight 4053 Da; Molecular weight distribution: 1.49; The viscosity of xylene at 60% solids is 5.96 cst; The hydroxyl content is 1.10%; M / Q is 0.92; The vinyl content is 2.6%; Light transmittance: 99.8%; Acid value: 12ppm.

[0031] Example 2 The difference between this embodiment and embodiment 1 is that the density of the water glass solution is 1.25 g / cm 3 , modulus is 3.3, silicon dioxide content is 8%; the acid catalyst is hydrochloric acid, wherein water: water glass solution: catalyst = 4:2.5:2; the end-capping agent is methyl end-capping agent and vinyl end-capping agent, the methyl end-capping agent is hexamethyldisiloxane, and the vinyl end-capping agent is 1,3-divinyltetramethyldisiloxane; the solvent is ethanol, and the end-capping agent: solvent = 1:5.

[0032] First, open the acid catalyst feed valve, and then close the acid catalyst feed valve 30 seconds after the acid catalyst is added; 5 minutes later, open the reactor stirring device, and the speed of the reactor stirring device is 250 r / min; open the water glass solution feed valve, and then close the water glass solution feed valve 30 seconds after the water glass solution is added, and the hydrolysis reaction time of the water glass solution under the action of the acid catalyst is 80 seconds; then open the end-capping agent feed valve, and then close the end-capping agent feed valve 30 seconds after the end-capping agent is added; control the temperature of the reactor heat exchange jacket to 45°C, stop the reactor heat exchange jacket after 0.75h, and close the reactor stirring device after reacting for 2.5h.

[0033] After standing for 30 minutes, the reactor wastewater discharge valve was fully opened and the intelligent sight glass was used for detection. The medium density was 0.825 g / cm 3 Then close the reactor wastewater discharge valve, let it stand for 15 minutes, and adjust the opening of the reactor wastewater discharge valve to 35% again. The medium density is 0.825g / cm 3 Then close the reactor wastewater discharge valve, let it stand for 15 minutes, and adjust the opening of the reactor wastewater discharge valve to 35% again. Repeat the above steps 3 times until the density data stabilizes at 0.825g / cm 3 Then close the reactor wastewater discharge valve; then open the first mixer discharge valve.

[0034] Among them, the temperature of the first mixer is controlled at 30°C, the flow rate of the oil phase flowing into the first mixer is 35g / s, and the flow rate of the acid catalyst flowing into the first mixer is 5 g / s; after the oleic acid mixture passes through the first mixer, the discharge valve at the lower end of the first mixer is opened, and the material is transferred to the first stratification tank for standing for oil-water separation. The temperature of the first stratification tank is controlled at 25°C. When the liquid level of the first stratification tank reaches 27%, the upper discharge valve of the first stratification tank is opened, and the opening of the upper discharge valve of the first stratification tank is controlled so that the flow rate of the first oil phase is 35g / s; the lower discharge valve of the first stratification tank is opened, and the opening of the lower discharge valve of the first stratification tank is controlled so that the flow rate of the wastewater in the first stratification tank is 5 g / s.

[0035] Among them, the temperature of the second mixer is controlled to be 50°C, the flow rate of the first oil phase in the first stratification tank flowing into the second mixer is 35g / s, and the flow rate of the salt washing reagent flowing into the second mixer is 10g / s; after the oil-water mixture passes through the second mixer, the discharge valve at the lower end of the second mixer is opened to transfer the material to the second stratification tank for standing for oil-water separation, and the temperature of the second stratification tank is controlled at 45°C. When the liquid level of the second stratification tank reaches 33%, the upper discharge valve of the second stratification tank is opened, and the opening of the upper discharge valve of the second stratification tank is controlled so that the flow rate of the second oil phase is 35g / s; the lower discharge valve of the second stratification tank is opened, and the opening of the lower discharge valve of the second stratification tank is controlled so that the flow rate of the waste water in the second stratification tank is 10g / s.

[0036] Among them, the temperature of the third mixer is controlled at 35°C, the flow rate of the second oil phase in the second stratification tank flowing into the third mixer is 35g / s, and the flow rate of the alkaline washing agent flowing into the third mixer is 17 g / s; after the oil-water mixture passes through the third mixer, the discharge valve at the lower end of the third mixer is opened, and the material is transferred to the third stratification tank for standing for oil-water separation. The temperature of the third stratification tank is controlled at 32°C. When the liquid level of the third stratification tank reaches 33%, the upper discharge valve of the third stratification tank is opened, and the opening of the upper discharge valve of the third stratification tank is controlled so that the flow rate of the third oil phase is 35g / s; the lower discharge valve of the third stratification tank is opened, and the opening of the lower discharge valve of the third stratification tank is controlled so that the flow rate of the waste water in the third stratification tank is 15g / s.

[0037] Among them, the temperature of the fourth mixer is controlled to be 50°C, the flow rate of the third oil phase in the third stratification tank flowing into the fourth mixer is 35g / s, and the flow rate of desalted water flowing into the fourth mixer is 17 g / s; after the oil-water mixture passes through the third mixer, the discharge valve at the lower end of the fourth mixer is opened, and the material is transferred to the fourth stratification tank for standing for oil-water separation. The temperature of the fourth stratification tank is controlled at 45°C. When the liquid level of the fourth stratification tank reaches 33%, the upper discharge valve of the fourth stratification tank is opened, and the opening of the upper discharge valve of the fourth stratification tank is controlled so that the flow rate of the fourth oil phase is 35g / s; the lower discharge valve of the fourth stratification tank is opened, and the opening of the lower discharge valve of the fourth stratification tank is controlled so that the flow rate of the wastewater in the fourth stratification tank is 17 g / s.

[0038] Among them, the temperature in the drying kettle is 130°C, the drying time is 2h, the vacuum degree is 0.09MPa, and the stirring speed is 15rpm.

[0039] MQ silicone resin for leather manufacturing is obtained, with the general formula (Me 3 SiO 1 / 2 )a(Me 2 ViSiO 3 / 2 )b(SiO 4 / 2 )c; Among them: weight average molecular weight 5336 Da; Molecular weight distribution: 1.62; The viscosity of xylene at 60% solids is 12.78 cst; The hydroxyl content is 1.02%; M / Q is 0.97; The vinyl content is 3.0%; Light transmittance: 99.8%; Acid value: 4ppm.

[0040] Example 3 The difference between this embodiment and embodiment 1 is that the density of the water glass solution is 1.5 g / cm 3 , modulus is 3.6, silicon dioxide content is 10%; the acid catalyst is phosphoric acid or p-toluenesulfonic acid, wherein water: water glass solution: catalyst = 4:3:2; the end-capping agent is methyl end-capping agent and vinyl end-capping agent, the methyl end-capping agent is trimethylchlorosilane, and the vinyl end-capping agent is dimethylvinylethoxysilane; the solvent is either isopropanol or ethanol, and the end-capping agent: solvent = 1:6.

[0041] First, open the acid catalyst feed valve, and then close the acid catalyst feed valve 30s after the acid catalyst is added; open the reactor stirring device 5min later, and the speed of the reactor stirring device is 300 r / min; open the water glass solution feed valve, and then close the water glass solution feed valve 30s after the water glass solution is added, and the hydrolysis reaction time of the water glass solution under the action of the acid catalyst is 30s; then open the end-capping agent feed valve, and then close the end-capping agent feed valve 30s after the end-capping agent is added; control the temperature of the reactor heat exchange jacket to 45°C, stop the reactor heat exchange jacket after 1.0h, and close the reactor stirring device after 3h of reaction.

[0042] After standing for 30 minutes, the reactor wastewater discharge valve was fully opened and the intelligent sight glass was used for detection. The medium density was 0.85g / cm 3 Then close the reactor wastewater discharge valve, let it stand for 20 minutes, and adjust the opening of the reactor wastewater discharge valve to 50% again. The medium density is 0.85g / cm 3 Then close the reactor wastewater discharge valve, let it stand for 20 minutes, and adjust the opening of the reactor wastewater discharge valve to 50% again. Repeat the above steps 3 times until the density data stabilizes at 0.8~0.85g / cm 3 Then close the reactor wastewater discharge valve; then open the first mixer discharge valve.

[0043] Among them, the temperature of the first mixer is controlled to be 40°C, the flow rate of the oil phase flowing into the first mixer is 50g / s, and the flow rate of the acid catalyst flowing into the first mixer is 5 g / s; after the oleic acid mixture passes through the first mixer, the discharge valve at the lower end of the first mixer is opened, and the material is transferred to the first stratification tank for standing for oil-water separation. The temperature of the first stratification tank is controlled at 30°C. When the liquid level of the first stratification tank reaches 30%, the upper discharge valve of the first stratification tank is opened, and the opening of the upper discharge valve of the first stratification tank is controlled so that the flow rate of the first oil phase is 50g / s; the lower discharge valve of the first stratification tank is opened, and the opening of the lower discharge valve of the first stratification tank is controlled so that the flow rate of the wastewater in the first stratification tank is 5g / s.

[0044] Among them, the temperature of the second mixer is controlled to be 50°C, the flow rate of the first oil phase in the first stratification tank flowing into the second mixer is 50g / s, and the flow rate of the salt washing reagent flowing into the second mixer is 15 g / s; after the oil-water mixture passes through the second mixer, the discharge valve at the lower end of the second mixer is opened to transfer the material to the second stratification tank for standing for oil-water separation, and the temperature of the second stratification tank is controlled at 45°C. When the liquid level of the second stratification tank reaches 35%, the upper discharge valve of the second stratification tank is opened, and the opening of the upper discharge valve of the second stratification tank is controlled so that the flow rate of the second oil phase is 50g / s; the lower discharge valve of the second stratification tank is opened, and the opening of the lower discharge valve of the second stratification tank is controlled so that the flow rate of the wastewater in the second stratification tank is 15g / s.

[0045] Among them, the temperature of the third mixer is controlled to be 60°C, the flow rate of the second oil phase in the second stratification tank flowing into the third mixer is 50g / s, and the flow rate of the alkaline washing agent flowing into the third mixer is 25 g / s; after the oil-water mixture passes through the third mixer, the discharge valve at the lower end of the third mixer is opened, and the material is transferred to the third stratification tank for standing for oil-water separation. The temperature of the third stratification tank is controlled at 55°C. When the liquid level of the third stratification tank reaches 35%, the upper discharge valve of the third stratification tank is opened, and the opening of the upper discharge valve of the third stratification tank is controlled so that the flow rate of the third oil phase is 50g / s; the lower discharge valve of the third stratification tank is opened, and the opening of the lower discharge valve of the third stratification tank is controlled so that the flow rate of the waste water in the third stratification tank is 25g / s.

[0046] Among them, the temperature of the fourth mixer is controlled to be 60°C, the flow rate of the third oil phase in the third stratification tank flowing into the fourth mixer is 50g / s, and the flow rate of desalted water flowing into the fourth mixer is 25 g / s; after the oil-water mixture passes through the third mixer, the discharge valve at the lower end of the fourth mixer is opened, and the material is transferred to the fourth stratification tank for standing for oil-water separation. The temperature of the fourth stratification tank is controlled at 55°C. When the liquid level of the fourth stratification tank reaches 35%, the upper discharge valve of the fourth stratification tank is opened, and the opening of the upper discharge valve of the fourth stratification tank is controlled so that the flow rate of the fourth oil phase is 50g / s; the lower discharge valve of the fourth stratification tank is opened, and the opening of the lower discharge valve of the fourth stratification tank is controlled so that the flow rate of the wastewater in the fourth stratification tank is 25g / s.

[0047] The temperature in the drying kettle was 180°C, the drying time was 1 h, the vacuum degree was 0.1 MPa, and the stirring speed was 50 rpm.

[0048] MQ silicone resin for leather manufacturing is obtained, with the general formula (Me 3 SiO 1 / 2 )a(Me 2 ViSiO 3 / 2 )b(SiO 4 / 2 )c; Among them: weight average molecular weight 4535 Da; Molecular weight distribution: 1.56; The viscosity of xylene at 60% solids is 6.97 cst; The hydroxyl content is 1.12%; M / Q is 0.95; The vinyl content is 2.77%; Light transmittance: 99.6%; Acid value: 7ppm.

[0049] Comparative Example 1 The difference between this comparative example and Example 1 is that the DCS linkage controller controls the temperature of the acid catalyst storage tank, the solvent storage tank, the water glass solution storage tank and the end-capping agent storage tank at 5°C.

[0050] MQ silicone resin for leather manufacturing is obtained, with the general formula (Me 3 SiO 1 / 2 )a(Me 2 ViSiO 3 / 2 )b(SiO 4 / 2 )c; Among them: weight average molecular weight 3699 Da; Molecular weight distribution: 1.42; The viscosity of xylene at 60% solids is 5.39 cst; The hydroxyl content is 0.78%; M / Q is 0.91; The vinyl content is 2.68%; Light transmittance: 99.8%; Acid value: 10ppm.

[0051] Comparative Example 2 The difference between this comparative example and Example 1 is that the DCS linkage controller controls the temperature of the acid catalyst storage tank, the solvent storage tank, the water glass solution storage tank and the end-capping agent storage tank at 20°C.

[0052] MQ silicone resin for leather manufacturing is obtained, with the general formula (Me 3 SiO 1 / 2 )a(Me 2 ViSiO 3 / 2 )b(SiO 4 / 2 )c; Among them: weight average molecular weight 5250Da; Molecular weight distribution: 1.58; The viscosity of xylene at 60% solids is 8.96 cst; The hydroxyl content is 1.22%; M / Q is 0.79; The vinyl content is 2.43%; Light transmittance: 99.6%; Acid value: 15ppm.

[0053] Comparative Example 3 The difference between this comparative example and Example 1 is that the DCS linkage controller controls the temperature of the heat exchange jacket of the reactor to be 35°C.

[0054] MQ silicone resin for leather manufacturing is obtained, with the general formula (Me 3 SiO 1 / 2 )a(Me 2 ViSiO 3 / 2 )b(SiO 4 / 2 )c; Among them: weight average molecular weight 5425Da; Molecular weight distribution: 1.66; The viscosity of xylene at 60% solids is 9.32 cst; The hydroxyl content is 1.04%; M / Q is 0.91; The vinyl content is 2.66%; Light transmittance: 98.0%; Acid value: 13ppm.

[0055] Comparative Example 4 The difference between this comparative example and Example 1 is that the temperature of the first mixer is controlled to be 30° C. The flow rate of the oil phase flowing into the first mixer is 60 g / s, and the flow rate of the acid catalyst flowing into the first mixer is 15 g / s.

[0056] MQ silicone resin for leather manufacturing is obtained, with the general formula (Me 3 SiO 1 / 2 )a(Me 2 ViSiO 3 / 2 )b(SiO 4 / 2 )c; Among them: weight average molecular weight 4165 Da; Molecular weight distribution: 1.46; The viscosity of xylene at 60% solid content is 6.12cst; The hydroxyl content is 0.78%; M / Q is 0.90; The vinyl content is 2.66%; Light transmittance: 99.7%; Acid value: 8ppm.

[0057] Comparative Example 5 The difference between this comparative example and Example 3 is that the temperature of the first mixer is controlled to be 30° C. The flow rate of the oil phase flowing into the first mixer is 60 g / s, and the flow rate of the acid catalyst flowing into the first mixer is 3 g / s.

[0058] MQ silicone resin for leather manufacturing is obtained, with the general formula (Me 3 SiO 1 / 2 )a(Me 2 ViSiO 3 / 2 )b(SiO 4 / 2 )c; Among them: weight average molecular weight 4699Da; Molecular weight distribution: 1.54; The viscosity of xylene at 60% solids is 7.41 cst; The hydroxyl content is 1.78%; M / Q is 0.89; Vinyl content is 2.55%; Light transmittance: 99.6%; Acid value: -12ppm.

[0059] Comparative Example 6 The difference between this comparative example and Example 3 is that the temperature of the second mixer is controlled to be 50° C. The flow rate of the first oil phase flowing into the second mixer is 50 g / s, and the flow rate of the salt washing agent flowing into the second mixer is 5 g / s.

[0060] MQ silicone resin for leather manufacturing is obtained, with the general formula (Me 3 SiO 1 / 2 )a(Me 2 ViSiO 3 / 2 )b(SiO 4 / 2 )c; Among them: weight average molecular weight 4831 Da; Molecular weight distribution: 1.54; The viscosity of xylene at 60% solids is 7.87 cst; The hydroxyl content is 1.01%; M / Q is 0.95; The vinyl content is 2.53%; Light transmission: 97.6%; Acid value: 24ppm.

[0061] Comparative Example 7 The difference between this comparative example and Example 3 is that the temperature of the second mixer is controlled to be 85° C., the flow rate of the first oil phase in the first stratification tank flowing into the second mixer is 60 g / s, and the flow rate of the salt washing agent flowing into the second mixer is 30 g / s.

[0062] MQ silicone resin for leather manufacturing is obtained, with the general formula (Me 3 SiO 1 / 2 )a(Me 2 ViSiO 3 / 2 )b(SiO 4 / 2 )c; Among them: weight average molecular weight 4860 Da; Molecular weight distribution: 1.53; The viscosity of xylene at 60% solids is 8.21 cst; The hydroxyl content is 1.03%; M / Q is 0.94; The vinyl content is 2.57%; Light transmittance: 96.7%; Acid value: 4ppm.

[0063] Comparative Example 8 The difference between this comparative example and Example 3 is that the temperature of the second mixer is controlled to be 15° C., the flow rate of the first oil phase in the first stratification tank flowing into the second mixer is 50 g / s, and the flow rate of the salt washing agent flowing into the second mixer is 10 g / s.

[0064] MQ silicone resin for leather manufacturing is obtained, with the general formula (Me 3 SiO 1 / 2 )a(Me 2 ViSiO 3 / 2 )b(SiO 4 / 2 )c; Among them: weight average molecular weight 4789 Da; Molecular weight distribution: 1.53; The viscosity of xylene at 60% solids is 7.55 cst; The hydroxyl content is 0.98%; M / Q is 0.90; The vinyl content is 2.52%; Light transmittance: 98.0%; Acid value: 23ppm.

[0065] Comparative Example 9 The difference between this comparative example and Example 3 is that the temperature of the third mixer is controlled to be 75° C., the flow rate of the second oil phase in the second stratification tank flowing into the third mixer is 60 g / s, and the flow rate of the alkaline washing agent flowing into the third mixer is 25 g / s.

[0066] MQ silicone resin for leather manufacturing is obtained, with the general formula (Me 3 SiO 1 / 2 )a(Me 2ViSiO 3 / 2 )b(SiO 4 / 2 )c; Among them: weight average molecular weight 4805 Da; Molecular weight distribution: 1.53; The viscosity of xylene at 60% solids is 7.71 cst; The hydroxyl content is 1.12%; M / Q is 0.88; The vinyl content is 2.48%; Light transmittance: 99.8%; Acid value: 0ppm.

[0067] Comparative Example 10 The difference between this comparative example and Example 3 is that the temperature of the third mixer is controlled to be 15° C., the flow rate of the second oil phase in the second stratification tank flowing into the third mixer is 60 g / s, and the flow rate of the alkaline washing agent flowing into the third mixer is 10 g / s.

[0068] MQ silicone resin for leather manufacturing is obtained, with the general formula (Me 3 SiO 1 / 2 )a(Me 2 ViSiO 3 / 2 )b(SiO 4 / 2 )c; Among them: weight average molecular weight 4784 Da; Molecular weight distribution: 1.53; The viscosity of xylene at 60% solids is 7.95 cst; The hydroxyl content is 1.05%; M / Q is 0.83; The vinyl content is 2.56%; Light transmittance: 97.8%; Acid value: 62ppm.

[0069] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. Any simple modification or equivalent change made to the above embodiment based on the technical essence of the present invention shall fall within the protection scope of the present invention.

Claims

1. An MQ silicone resin suitable for leather manufacturing, characterized in that: The general formula is (Me3SiO 1 / 2 )a(Me2ViSiO 3 / 2 )b(SiO 4 / 2 )c; Having the structural formula: Among them: weight average molecular weight 4000~5500 Da; Molecular weight distribution 1.3~2.0; The viscosity of xylene with 60% solid content is 5~15cst; The hydroxyl content is 0.5~2%; M / Q is 0.9~1.0; Vinyl content is 2.0~3.0%; Light transmittance: 99%~100%; Acid value: 0~20 ppm.

2. The MQ silicone resin suitable for leather manufacturing according to claim 1, characterized in that: In the general formula, a=15~30; b=3~10; c=20~30.

3. An industrial control method for MQ silicone resin suitable for leather manufacturing according to claim 1 or 2, characterized in that: Using water glass and pure water as raw materials, a hydrolysis reaction is carried out in a reactor under the action of an acid catalyst, and then a capping agent and a solvent are added to carry out a capping reaction. After standing for oil-water separation, the first oil phase flows into a first mixer, and an acid catalyst is added to the first mixer for pickling. After the pickling is completed, the first oil-liquid separation is carried out, and the second oil phase flows into a second mixer, and a salt washing agent is added to the second mixer for salt washing. After the salt washing is completed, the second oil-liquid separation is carried out, and the third oil phase flows into a third mixer, and an alkali washing agent is added to the third mixer for alkali washing. After the alkali washing is completed, the third oil-liquid separation is carried out, and the fourth oil phase flows into a fourth mixer, and desalted water is added to the fourth mixer for water washing. After the water washing is completed, the fourth oil-liquid separation is carried out, and the fifth oil phase flows into a drying kettle for drying treatment; During the reaction process, at least the following control methods are included: (I) The DCS interlock controller controls the temperature of the acid catalyst storage tank, solvent storage tank, water glass solution storage tank and end-capping agent storage tank; (II) The DCS linkage controller controls the opening and closing of the acid catalyst diaphragm pump, the opening and closing of the water glass solution diaphragm pump, the opening and closing of the end-capping agent diaphragm pump, the opening and closing of the acid catalyst feed valve, the opening and closing of the water glass solution feed valve, the opening and closing of the end-capping agent feed valve, the opening and closing of the solvent feed valve and the opening and closing of the reactor discharge valve; (III) The DCS linkage controller controls the opening and closing of the reactor stirring device, the speed of the reactor stirring device, the time of the end-capping reaction and the temperature of the reactor heat exchange jacket; (IV) The DCS linkage controller controls the temperature of the first mixer, the flow rate of the oil phase flowing into the first mixer, the flow rate of the acid catalyst flowing into the first mixer, and the opening and closing of the discharge valve of the first mixer; (V), the DCS linkage controller controls the temperature of the second mixer, the flow rate of the first oil phase into the second mixer, the flow rate of the salt washing reagent into the second mixer, and the opening and closing of the discharge valve of the second mixer; (VI), a DCS linkage controller controls the temperature of the third mixer, the flow rate of the second oil phase flowing into the third mixer, the flow rate of the alkali washing agent flowing into the third mixer, and the opening and closing of the discharge valve of the third mixer; (VII), the DCS linkage controller controls the temperature of the fourth mixer, the flow rate of the third oil phase flowing into the fourth mixer, the flow rate of the water washing reagent flowing into the fourth mixer, and the opening and closing of the discharge valve of the fourth mixer; (VIII) The DCS linkage controller controls the temperature, drying time, vacuum degree and stirring speed in the drying kettle.

4. The industrial control method of MQ silicone resin suitable for leather manufacturing according to claim 3, characterized in that: The DCS interlock controller controls the temperature of the acid catalyst storage tank, solvent storage tank, water glass solution storage tank and end-capping agent storage tank at 5~25℃. When the storage tank temperature is lower than 7℃, the DCS control system automatically controls the storage tank heat exchange jacket to open the hot water circulation switch valve; when the storage tank temperature is higher than 23℃, the DCS control system controls the storage tank heat exchange jacket to open the cold water circulation switch valve; the density of the water glass solution is 1.0~1.5g / cm 3 , modulus is 3.0~3.6, silicon dioxide content is 7~10%; the acid catalyst is selected from one of concentrated sulfuric acid, hydrochloric acid, phosphoric acid, and p-toluenesulfonic acid, wherein water: water glass solution: catalyst = 4:2~3:2; the end-capping agent is a methyl end-capping agent and a vinyl end-capping agent, the methyl end-capping agent is selected from any one of trimethylchlorosilane or hexamethyldisiloxane, and the vinyl end-capping agent is selected from any one of dimethylvinylethoxysilane or 1,3-divinyltetramethyldisiloxane; the solvent is selected from any one of isopropanol or ethanol, and the end-capping agent: solvent = 1:4~6.

5. The industrial control method of MQ silicone resin suitable for leather manufacturing according to claim 4, characterized in that: Start DCS linkage control, first open the acid catalyst feed valve, and close the acid catalyst feed valve 30s after the acid catalyst is added; open the reactor stirring device after 2~5min, and the speed of the reactor stirring device is 200~300 r / min; open the water glass solution feed valve, and close the water glass solution feed valve 30s after the water glass solution is added, and the hydrolysis reaction time of the water glass solution under the action of the acid catalyst is 0~80s; then open the end-capping agent feed valve, and close the end-capping agent feed valve 30s after the end-capping agent is added; control the temperature of the reactor heat exchange jacket to 30~60℃, stop the reactor heat exchange jacket after 0.5~2.0h, and close the reactor stirring device after 2~3h of reaction.

6. The industrial control method of MQ silicone resin suitable for leather manufacturing according to claim 5, characterized in that: After standing for 30 minutes, fully open the reactor wastewater discharge valve and use the smart mirror to check that the medium density is between 0.8 and 0.85 g / cm 3 Then close the reactor wastewater discharge valve, let it stand for 10-30 minutes, and adjust the opening of the reactor wastewater discharge valve to 25-50% again. The medium density is between 0.8-0.85 g / cm 3 Then close the reactor wastewater discharge valve, let it stand for 10-30 minutes, and adjust the opening of the reactor wastewater discharge valve to 25-50% again. Repeat the above steps 3 times until the density data stabilizes at 0.8-0.85 g / cm 3 Then close the reactor wastewater discharge valve; then open the first mixer discharge valve.

7. The industrial control method of MQ silicone resin suitable for leather manufacturing according to claim 6, characterized in that: The temperature of the first mixer is controlled at 10-50°C, the flow rate of the oil phase flowing into the first mixer is 30-60g / s, and the flow rate of the acid catalyst flowing into the first mixer is 5-10 g / s; after the oleic acid mixture passes through the first mixer, the discharge valve at the lower end of the first mixer is opened, and the material is transferred to the first stratification tank for standing for oil-water separation. The temperature of the first stratification tank is controlled at 10-40°C. When the liquid level of the first stratification tank reaches 25-30%, the upper discharge valve of the first stratification tank is opened, and the opening of the upper discharge valve of the first stratification tank is controlled so that the flow rate of the first oil phase is 30-60g / s; the lower discharge valve of the first stratification tank is opened, and the opening of the lower discharge valve of the first stratification tank is controlled so that the flow rate of the waste acid in the first stratification tank is 5-10 g / s.

8. The industrial control method of MQ silicone resin suitable for leather manufacturing according to claim 7, characterized in that: The temperature of the second mixer is controlled at 20-80°C, the flow rate of the first oil phase in the first stratification tank flowing into the second mixer is 30-60 g / s, and the flow rate of the salt washing reagent flowing into the second mixer is 5-20 g / s; after the oil-water mixture passes through the second mixer, the discharge valve at the lower end of the second mixer is opened to transfer the material to the second stratification tank for standing for oil-water separation, and the temperature of the second stratification tank is controlled at 20-60°C. When the liquid level of the second stratification tank reaches 30-35%, the upper discharge valve of the second stratification tank is opened, and the opening of the upper discharge valve of the second stratification tank is controlled so that the flow rate of the second oil phase is 30-60 g / s; the lower discharge valve of the second stratification tank is opened, and the opening of the lower discharge valve of the second stratification tank is controlled so that the flow rate of the wastewater in the second stratification tank is 5-20 g / s.

9. The industrial control method of MQ silicone resin suitable for leather manufacturing according to claim 8, characterized in that: The temperature of the third mixer is controlled at 20-70°C, the flow rate of the second oil phase in the second stratification tank flowing into the third mixer is 30-60 g / s, and the flow rate of the alkaline washing agent flowing into the third mixer is 10-30 g / s; after the oil-water mixture passes through the third mixer, the discharge valve at the lower end of the third mixer is opened, and the material is transferred to the third stratification tank for standing for oil-water separation. The temperature of the third stratification tank is controlled at 20-60°C. When the liquid level of the third stratification tank reaches 30-35%, the upper discharge valve of the third stratification tank is opened, and the opening of the upper discharge valve of the third stratification tank is controlled so that the flow rate of the third oil phase is 30-60 g / s; the lower discharge valve of the third stratification tank is opened, and the opening of the lower discharge valve of the third stratification tank is controlled so that the flow rate of the waste water in the third stratification tank is 10-30 g / s.

10. The industrial control method of MQ silicone resin suitable for leather manufacturing according to claim 9, characterized in that: The temperature of the fourth mixer is controlled at 20-80°C, the flow rate of the third oil phase in the third stratification tank flowing into the fourth mixer is 30-60 g / s, and the flow rate of desalted water flowing into the fourth mixer is 10-30 g / s; after the oil-water mixture passes through the third mixer, the discharge valve at the lower end of the fourth mixer is opened, and the material is transferred to the fourth stratification tank for standing for oil-water separation, and the temperature of the fourth stratification tank is controlled at 20-50°C. When the liquid level of the fourth stratification tank reaches 30-35%, the upper discharge valve of the fourth stratification tank is opened, and the opening of the upper discharge valve of the fourth stratification tank is controlled so that the flow rate of the fourth oil phase is 30-60 g / s; the lower discharge valve of the fourth stratification tank is opened, and the opening of the lower discharge valve of the fourth stratification tank is controlled so that the flow rate of the wastewater in the fourth stratification tank is 10-30 g / s.

11. The industrial control method of MQ silicone resin suitable for leather manufacturing according to claim 10, characterized in that: The temperature in the drying kettle is 80~180℃, the drying time is 1~3h, the vacuum degree is 0.08~0.1 MPa, and the stirring speed is 10~50 rpm.

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