Method for preparing polyquaternium-10

Abstract

The invention discloses a method for preparing polyquaternium-10, which comprises the following steps: (1) dispersion: adding an organic solvent into a reactor, adding hydroxyethyl cellulose under a stirring condition, and fully dispersing; (2) alkalization: adding an aqueous solution of alkali and alkalescence ionic liquid serving as an auxiliary alkalizer into the hydroxyethyl cellulose mixed solution in the step (1) for alkalization treatment; (3) etherification reaction: adding a cationic etherifying agent into the mixed solution in the step (2) for reaction under rapid stirring; and (4) washing and purifying: filtering, washing, filtering, drying and crushing the substance obtained in the step (3) to obtain the polyquaternium-10. According to the method, the auxiliary basifier is added in the reaction to increase the phase interface of the solid-liquid heterogeneous reaction, so that the reaction efficiency is effectively improved, the generation of byproducts and the degradation of the raw material hydroxyethyl cellulose are reduced, the post-treatment difficulty is reduced, the raw material consumption and the energy consumption are reduced, and the obtained product is relatively high in nitrogen content, high in light transmittance and suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing polyquaternium-10, belonging to the field of cellulose modified derivatives. Background technique [0002] Polyquaternium-10 is a cationic modified derivative of hydroxyethyl cellulose, which is often used in personal care cationic conditioners. Due to its unique structure, it is very good for the cuticle of human skin and hair. Nursing and protective effect, is used in various daily chemical products. As a water-soluble cationic polymer compound, it can be compatible with a variety of non-ionic, anionic and cationic surfactants to promote the deposition of active ingredients on the hair, protect and nourish the hair, and is widely used in shampoo and hair care products , play the role of antistatic, moisturizing and supple. For polyquaternium-10 products, nitrogen content and light transmittance are important indicators. Nitrogen content corresponds to the degree of cationization of cellulose. Currentl...

AI Technical Summary

Problems solved by technology

[0003] At present, most of the production of polyquaternium-10 adopts wet process, under the dispersion of alcohol aqueous solution and alkalization of lye, cationic etherification agent is used It is prepared by replacing the active hydrogen on hydroxyethyl cellulose. The advantages of this method are uniform reaction, mild conditions, and easy operation. However, because the reaction is a solid-liquid heterogeneous reaction, the lye cannot fully contact the hydroxyl group under the dispersion of alcohol aqueous solution. The active hydrogen of ethyl cellulose is used to alkalize it, and the etherification agent will have a side reaction with the lye in the alcoholic water phase, resulting in low etherification reaction efficiency, low cationic substitution degree, and low nitrogen content in the product. The increase in side reactions leads to high impurity content, and there are also problems such as large solvent usage and long post-treatment cycle

For example, the cationic cellulose products produced by a single wet process in the patent US4228277 have problems such as low cationic substitution degree and unstable substitution amount, which affect the end use of the product

Patent WO01 / 48021 uses a secondary wet reaction. On the basis of the first reaction, the product with nitrogen content is reacted again, thereby improving the cationic substitution degree and nitrogen content of the product, but the secondary reaction consumes more solvent and raw materials. The quantity is large, and the process is difficult, the operation is complicated, the cost is high, and it is not suitable for production

In the patent CN1944464A, the process of dry reaction first and then wet reaction is adopted. First, alkalization with lye in a solid state and mixed etherification agent are used for dry reaction, followed by a wet reaction. Compared with the two The sub-wet reaction reduces the consumption of solvent and obtains a product with a higher degree of substitution, but increases the complexity of the process, especially the dry reaction will make the reaction less uniform, increase the difficulty of post-processing, and lengthen the cycle. The obtained product has the problem that the light transmittance is not high enough, which affects the end use of the product

Patent CN102268096A adopts a one-time wet reaction process, which uses a strong alkaline sodium borate reagent as an activator. Due to the activation of sodium borate, a product with a higher cationic substitution is obtained, but it also comes from The increase in the amount of alkali used in the system will increase the side reactions involved in the cationic etherification agent, and the consumption of raw materials will be large. The amount required for the cationic etherification agent is 3-4 times that of cellulose. The increase in reaction will also make the product post-processing more complicated

[0004] In summary, the current production process for preparing polyquaternium-10 products with a high degree of cationic substitution is insufficient in the degree of cationization or etherification in a single reaction The consumption of reagent is relatively large, the method of multiple reactions is complex or the consumption of raw materials and solvents is large, and the production cost is high. The reason is that the production process of polyquaternium-10 involves multiphase reactions, mainly solid Liquid phase reaction, the mass transfer between the phases of the current production process is not sufficient, therefore, it is necessary to find a new process to fully increase the reaction phase interface to solve various deficiencies in the existing technology

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