Preparation technology of crude amino silicone oil

Abstract

The invention relates to the field of preparation of silicone oil, in particular to a preparation technology of crude amino silicone oil with relatively high molecular weight uniformity. The preparation technology comprises the following preparation steps: 1), premixing raw materials: premixing mixed dimethylcyclosiloxane and an end-capping agent to obtain a premix I, and premixing a coupling agent and a solid catalyst to obtain a premix II; 2), placing the premix I and the premix II which are obtained in the step 1) in a container, and performing polycondensation to obtain a polycondensationreaction product, wherein during the polycondensation, the reaction temperature is controlled to be 100-200 DEG C; 3), performing reduced pressure distillation on the polycondensation reaction productobtained in the step 2), completing the distillation till the mass tends to be constant, and lowering the temperature to 40 DEG C or below to obtain the crude amino silicone oil.

Description

technical field [0001] The invention relates to the field of silicone oil preparation, in particular to a preparation process of amino silicone oil crude oil with high molecular weight uniformity. Background technique [0002] Ammonia-based modified silicone oil can be regarded as the product after part of the methyl groups (including side and end positions) in dimethyl silicone oil are substituted by amino-hydrocarbon groups. Ammonia-based silicone oil retains the original hydrophobicity and desorption properties of dimethyl silicone oil. In addition to modulus, the presence of aminohydrocarbon groups can also give it reactivity, adsorption, lubricity and softness, so it has been widely used in fabric softening agents, polishing machines, coating additives and resin modifiers. And become one of the varieties with the largest amount of carbon functional group silicone oil. [0003] However, due to the process and raw materials in the prior art, that is, it is difficult to c...

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Problems solved by technology

[0003] However, due to the process and raw materials in the prior art, that is, it is difficult to control the position of the ring opening and the length of the molecular chain formed by condensation or polymerization when the ring opening, condensation and polymerization reactions occur in production, the amino silicone oil obtained in the same batch of production is condensed. , The degree of polymerization is high or low, and the molecular weight uniformity is low. It is often composed of amino silicone oil with relatively large molecular weight and amino silicone oil with small molecular weight, and mixed with a large amount of impurities.

[0004] For example, the book "Organosilicon Chemistry and Technology" edited by Lai Guoqiao and others introduces the traditional alkali-catalyzed equilibrium method to prepare amino silicone oil. 4 and 1,3-diaminopropyl-1,1,3,3-tetramethyldisiloxane under the catalysis of potassium hydroxide strong base to prepare amino silicone oil, but the amount of potassium hydroxide is large, the reaction time is long, condensation, The distribution range of the degree of polymerization is large, and the molecular weight uniformity of the formed amino silicone oil is very low. To improve these aspects, it is necessary to add the accelerator cyclohexyl-18-crown ether-6 as an accelerator, but the complexity of the process increases, and the raw material higher control requirements

[0005] Another example is the preparation of amino silicone oil by the traditional hydrosilicon addition method recorded in "Organosilicon Chemistry and Technology". 2 SiO) n SiMe 2 H and CH 2 =CMeCH 2 NHEt (allylamine) undergoes addition polymerization under the coordination catalysis of hexachloroplatinic acid, in which the amino group of allylamine needs to be protected, otherwise a large number of side reactions will occur, resulting in a substantial increase in impurity content, and the degree of polymerization of amino silicone oil produced Both are low, unable to produce amino silicone oil with larger molecular weight

[0006] Also as the process of preparing amino silicone oil by traditional condensation method recorded in "Organosilicon Chemistry and Technology", it uses H 2 NC 3 h 6 MeSi(OMe) 2 or H 2 NC 3 h 6 Si(OMe) 3 and HO(Me 4 SiO) n H undergoes a dealcoholization condensation reaction to obtain a double-ended aminohydrocarbon-based silicone oil. Although it has the advantages of low reaction temperature and fast reaction speed, the molecular weight uniformity of the amino silicone oil produced by it is poor, and the alcohols produced are in the reaction process. It is an impurity that is difficult to completely remove and reduces product quality

[0007] In addition, the traditional method of preparing amino silicone oil recorded in the book "Organosilicon Chemistry and Technology" also includes: using methylaminopropyl dimethoxysilane as raw material, using NH 2 C 3 h 6 SiMe(OMe) 2 、D 4 Co-catalyzed equilibrium reaction with MM with basic catalyst to prepare amino-propyl-containing amino silicone oil in side group; use methylaminopropyl dimethoxysilane hydrolyzate, with D 4 Equilibrium polymerization occurs with MM under the action of a basic catalyst to prepare the aminosilicone oil containing aminopropyl in the side group; with [Me(C 3 h 6 NHC 2 h 4 NH 2 )SiO] 4 As raw material, add [Me(C 3 h 6 NHC 2 h 4 NH 2 )-SiO] 4 , (Me 2 SiO) 4 and (Me 3 Si) 2 O carry out basic catalytic equilibrium reaction to prepare amino silicone oil with amino groups in side groups, but the above process methods cannot produce amino silicone oil with high degree of polymerization and uniform molecular weight distribution.

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