Synthesis process of novel anionic softener
By simplifying the synthesis process of anionic softener, using the mixing, heating, liquid separation and neutralization steps of specific raw materials and equipment, the production efficiency is improved and the antioxidant performance is achieved, and the complex process problems in the existing technology are solved.
Patent Information
- Application Number
- CN202510703909.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-29
- Publication Date
- 2025-09-02
AI Technical Summary
The existing anionic softener synthesis process is complicated, resulting in low production efficiency.
Using a new synthesis process of anionic softener, including mixing, heating, liquid separation, detection and neutralization, the use of specific raw materials and equipment simplifies the process flow and improves efficiency.
The synthesis of anionic softener with antioxidant and high efficiency is achieved, and the complex process problems in the prior art are solved.
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of softener synthesis technology, in particular to a synthesis technology of a novel anionic softener. Background Art
[0002] Softeners are chemicals that alter the static and dynamic coefficients of friction of fibers. Changing the static coefficient of friction creates a smoother feel, making it easier to move across the fiber or fabric. Changing the dynamic coefficient of friction facilitates the movement of the microstructure between fibers, making the fibers or fabric more easily deformable. The combined effect of these two factors is known as softness. Softeners are categorized by their ionicity into four types: cationic, nonionic, anionic, and amphoteric quaternary ammonium salts.
[0003] The existing synthesis process of anionic softeners is relatively complicated. The synthesis process involves two of the three major surfactant synthesis processes, namely esterification and sulfonation, as well as multiple technologies such as ester exchange, emulsion polymerization, and concentration. It uses more than 20 kinds of raw materials, resulting in a cumbersome production process and low efficiency. Summary of the Invention
[0004] (1) Technical problems solved
[0005] In view of the shortcomings of the existing technology, the present invention provides a new synthesis process of anionic softener, which has the advantages of anti-oxidation and high efficiency, and solves the problem that the synthesis process of the existing anionic softener is relatively complicated.
[0006] (2) Technical solution
[0007] To achieve the above object, the present invention provides the following technical solution: a synthesis process for a novel anionic softener, comprising the following steps: S1: preparing raw materials; S2: mixing palm oil, glycerin, sodium hydroxide, and an antioxidant in a mixing device; S3: heating the mixture while stirring until the mixture reacts for 2-4 hours; S4: allowing the mixture to stand for 48 hours using a liquid separator, and then discharging the lower layer of the mixture; S5: detecting the amount of residual glycerin, and completing the synthesis of glyceride when the residual glycerin is less than 2%; S6: mixing glyceride, aminosulfonic acid, urea, and an antioxidant in a mixing device; S7: heating the mixture while stirring until the mixture reacts for 4-8 hours; S8: detecting the concentration of anionic active substances and an infrared chromatogram; S9: after the mixture passes the test, adding sodium hydroxide for neutralization, the reaction temperature being below 70°C and the neutralization time being at least 3 hours; S10: removing the generated ammonia gas using nitrogen and passing it into an exhaust gas treatment device for absorption. After the ammonia gas is completely discharged, the sulfonation reaction of the glyceride is completed, and the neutralization process is considered to be complete.
[0008] In some embodiments, the raw materials in S1 include: castor oil, hydrogenated castor oil, beef tallow, hydrogenated beef tallow, soybean oil, hydrogenated soybean oil, palm oil, hydrogenated palm oil, glycerol, sodium hydroxide, glyceryl distearate, glyceryl dioleate, glyceryl monostearate, urea, and aminosulfonic acid.
[0009] In some embodiments, the heating temperature in S2 is 80-100°C, and the heating temperature in S7 is 80-100°C.
[0010] In some embodiments, the liquid separation device in S4 is a separating funnel.
[0011] (3) Beneficial effects
[0012] Compared with the prior art, the present invention provides a novel synthesis process of anionic softener, which has the following beneficial effects:
[0013] During the synthesis, palm oil, glycerol, sodium hydroxide and an antioxidant are mixed and heated through a mixing device until the reaction lasts for 2-4 hours. The mixture is allowed to stand for 48 hours using a separating funnel, and the lower layer material is discharged. When the residual glycerol is less than 2%, glyceride, aminosulfonic acid, urea and an antioxidant are mixed and heated through a mixing device. The concentration of anionic active substances and an infrared chromatogram are tested. If the concentration is qualified, sodium hydroxide is added for neutralization. Finally, nitrogen is used to remove the generated ammonia gas, which is then passed through an exhaust gas treatment device for absorption. After the ammonia gas is completely discharged, the sulfonation reaction of the glyceride is completed, and the neutralization process is considered to be completed. The invention has the advantages of anti-oxidation and high efficiency, and solves the problem that the synthesis process of the existing anionic softener is relatively complicated. DETAILED DESCRIPTION
[0014] It should be noted that all directional indications in the embodiments of the present application are only used to explain the relative position relationship, movement status, etc. between the components in a certain specific posture. If the specific posture changes, the directional indication will also change accordingly.
[0015] In this application, unless otherwise specified or limited, the terms "connection" and "fixation" should be understood in a broad sense. For example, "fixation" can mean fixed connection, detachable connection, or integration; mechanical connection or electrical connection; direct connection or indirect connection through an intermediate medium; internal communication between two elements or interaction between two elements, unless otherwise specified. For those skilled in the art, the specific meanings of the above terms in this application can be understood according to specific circumstances.
[0016] In addition, the descriptions of "first", "second", etc. in this application are for descriptive purposes only and should not be understood as indicating or implying their relative importance or implicitly indicating the number of the technical features indicated. Therefore, the features defined as "first" or "second" may explicitly or implicitly include at least one of such features. In addition, the technical solutions between the various embodiments can be combined with each other, but this must be based on the fact that they can be implemented by ordinary technicians in this field. When the combination of technical solutions is contradictory or cannot be implemented, it should be deemed that such combination of technical solutions does not exist and is not within the scope of protection required by this application.
[0017] In the related art, the synthesis process of anionic softening agent is as follows:
[0018] (1) Synthesis of sulfosuccinate
[0019] The synthesis is divided into two steps. The first step is to prepare maleate, based on which sodium sulfosuccinate is synthesized:
[0020]
[0021] Determination of esterification endpoint: acid value (mg KOH / g) ≤ 5.
[0022] Sulfonation endpoint determination: using the Epton method to determine the effective content of anionic active substances ≥ 60%.
[0023] Diester conversion rate: ≥96%.
[0024] The above is the synthesis of sodium dioctadecyl sulfosuccinate. The process for synthesizing monoester is similar to the above except that the feed ratio should be adjusted. The reaction formula is as follows:
[0025]
[0026] The sulfonation end point is still determined by the Epton method, with a content of ≥60%.
[0027] When used, monoester and diester are mixed in a mass ratio of 2:3. In actual production, since the synthesis process, catalyst and sulfonating agent of the two are the same, appropriate feeding is controlled.
[0028] The hydrophilic-lipophilic balance (HLB) values of monoesters and diesters are as follows:
[0029] Sulfonated succinic acid monoester 33.2
[0030] Sulfonated succinic acid diester 10.9
[0031] (2) Preparation of auxiliary surfactant
[0032] The synthesized sodium sulfosuccinate is difficult to dissolve and dilute at room temperature. It must be combined with a nonionic surfactant with good emulsification and dispersibility, and an anionic smoothing agent to improve water absorption and smoothness to produce an excellent anionic softener. Based on this, five varieties can be derived. The main raw material is sodium sulfosuccinate, and the main auxiliary materials are:
[0033] ①Synthesis of pentaerythritol ester: prepared by transesterification reaction
[0034] The molar ratio of hardened oil to pentaerythritol is important in this reaction. The reaction endpoint is controlled by the hydroxyl value, and the product is a mixture of monoesters and diesters.
[0035] ②Synthesis of sorbitan esters, the reaction formula is as follows:
[0036]
[0037] The product is also a mixture of mono- and diesters, and the end point is controlled by the acid value.
[0038] ③Anionic smoothing hy108A is an anionic silicone product with outstanding water absorption and smoothness. By mixing the above materials, you can make an anionic softener, which can be used for finishing cotton and knitwear.
[0039] The present application is described below with reference to specific embodiments:
[0040] Example 1
[0041] A synthesis process for a novel anionic softener comprises the following steps:
[0042] S1: prepare raw materials, including castor oil, hydrogenated castor oil, tallow, hydrogenated tallow, soybean oil, hydrogenated soybean oil, palm oil, hydrogenated palm oil, glycerol, sodium hydroxide, glyceryl distearate, glyceryl dioleate, glyceryl monostearate, urea, and aminosulfonic acid; S2: mix palm oil, glycerol, sodium hydroxide, and antioxidant through a mixing device; S3: heat the mixture while stirring at 80°C until the mixture reacts for 2 hours; S4: let the mixture stand for 48 hours using a separating funnel, and then discharge the lower layer of the mixture; S5: detect the amount of residual glycerol until the residual glycerol is less than 0. When the concentration of glycerol ester reaches 2%, the synthesis of glycerol ester is completed; S6: glycerol ester, aminosulfonic acid, urea, and antioxidant are mixed in a mixing device; S7: while stirring, heating is carried out at a temperature of 80°C until the reaction is carried out for 4 hours; S8: the concentration of anionic active substances and the infrared chromatogram are detected; S9: after the test is qualified, sodium hydroxide is added for neutralization, the reaction temperature is below 70°C, and the neutralization time is more than 3 hours; S10: nitrogen is used to remove the generated ammonia gas, and the gas is passed into an exhaust gas treatment device for absorption. After the ammonia gas is completely discharged, the sulfonation reaction of the glycerol ester is completed, and the neutralization process is considered to be completed.
[0043] Example 2
[0044] A synthesis process for a novel anionic softener comprises the following steps:
[0045] S1: prepare raw materials, including castor oil, hydrogenated castor oil, tallow, hydrogenated tallow, soybean oil, hydrogenated soybean oil, palm oil, hydrogenated palm oil, glycerol, sodium hydroxide, glyceryl distearate, glyceryl dioleate, glyceryl monostearate, urea, and aminosulfonic acid; S2: mix palm oil, glycerol, sodium hydroxide, and antioxidant through a mixing device; S3: heat the mixture while stirring at 90°C until the reaction lasts for 3 hours; S4: let the mixture stand for 48 hours using a separating funnel, and then discharge the lower layer of the mixture; S5: detect the amount of residual glycerol until the residual glycerol is less than 0.05. When the concentration of glycerol ester reaches 2%, the synthesis of glycerol ester is completed; S6: glycerol ester, aminosulfonic acid, urea, and antioxidant are mixed in a mixing device; S7: while stirring, heating is carried out at a temperature of 90°C until the reaction is carried out for 6 hours; S8: the concentration of anionic active substances and the infrared chromatogram are detected; S9: after the test is qualified, sodium hydroxide is added for neutralization, the reaction temperature is below 70°C, and the neutralization time is more than 3 hours; S10: nitrogen is used to remove the generated ammonia gas, and the gas is passed into an exhaust gas treatment device for absorption. After the ammonia gas is completely discharged, the sulfonation reaction of the glycerol ester is completed, and the neutralization process is considered to be completed.
[0046] Example 3
[0047] A synthesis process for a novel anionic softener comprises the following steps:
[0048] S1: prepare raw materials, including castor oil, hydrogenated castor oil, tallow, hydrogenated tallow, soybean oil, hydrogenated soybean oil, palm oil, hydrogenated palm oil, glycerol, sodium hydroxide, glyceryl distearate, glyceryl dioleate, glyceryl monostearate, urea, and aminosulfonic acid; S2: mix palm oil, glycerol, sodium hydroxide, and antioxidant through a mixing device; S3: heat the mixture while stirring at 100°C until the reaction lasts for 4 hours; S4: let the mixture stand for 48 hours using a separating funnel, and then discharge the lower layer of the mixture; S5: detect the amount of residual glycerol until the residual glycerol is less than 0. When the concentration of glycerol ester reaches 2%, the synthesis of glycerol ester is completed; S6: glycerol ester, aminosulfonic acid, urea, and antioxidant are mixed in a mixing device; S7: while stirring, heating is carried out at a heating temperature of 100°C until the reaction takes place for 8 hours; S8: the concentration of anionic active substances and the infrared chromatogram are detected; S9: after the test is qualified, sodium hydroxide is added for neutralization, the reaction temperature is below 70°C, and the neutralization time is more than 3 hours; S10: nitrogen is used to remove the generated ammonia gas, and the gas is passed into an exhaust gas treatment device for absorption. After the ammonia gas is completely discharged, the sulfonation reaction of the glycerol ester is completed, and the neutralization process is considered to be completed.
[0049] In the description of this specification, the description with reference to the terms "one embodiment", "some embodiments", "example", "specific example", or "some examples" means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present application. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner. In addition, those skilled in the art can combine and combine different embodiments or examples described in this specification.
[0050] In addition, the technical solutions between the various embodiments can be combined with each other, but they must be based on the fact that ordinary technicians in this field can implement them. When the combination of technical solutions is mutually contradictory or cannot be implemented, it should be deemed that such a combination of technical solutions does not exist and is not within the scope of protection required by this application.
[0051] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, and variations may be made to these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.
Claims
1. A novel synthesis process of anionic softener, characterized in that: The following steps are involved: S1: Prepare raw materials; S2: mixing palm oil, glycerin, sodium hydroxide and antioxidant through a mixing device; S3: While stirring, heat treatment is performed until the reaction lasts for 2-4 hours; S4: After the liquid separation device has been stationary for 48 hours, the lower layer of material is discharged; S5: Detecting the residual glycerol content until the residual glycerol is less than 2%, completing the synthesis of glyceride; S6: mixing the glyceride, aminosulfonic acid, urea, and antioxidant through a mixing device; S7: While stirring, heat treatment is performed until the reaction lasts for 4-8 hours; S8: Detection of anionic active substance concentration and infrared chromatogram; S9: After the test is qualified, add sodium hydroxide to neutralize, the reaction temperature is below 70 ° C, and the neutralization time is more than 3 hours; S10: Use nitrogen to remove the generated ammonia gas and pass it into the tail gas treatment device for absorption. After the ammonia gas is completely discharged, the sulfonation reaction of the glyceride is completed, and the neutralization process is considered to be completed.
2. The synthesis process of a novel anionic softener according to claim 1, characterized in that: The raw materials in S1 include: castor oil, hydrogenated castor oil, beef tallow, hydrogenated beef tallow, soybean oil, hydrogenated soybean oil, palm oil, hydrogenated palm oil, glycerol, sodium hydroxide, glyceryl distearate, glyceryl dioleate, glyceryl monostearate, urea, and aminosulfonic acid.
3. The synthesis process of a novel anionic softener according to claim 1, characterized in that: The heating temperature in S2 is 80-100°C, and the heating temperature in S7 is 80-100°C.
4. The synthesis process of a novel anionic softener according to claim 1, characterized in that: The liquid separation device in S4 is a separating funnel.