Efficient amino acid surfactant circular reaction device

Abstract

The utility model relates to an efficient amino acid surfactant circular reaction device which comprises a reaction kettle, the water injection pipe is connected into the reaction kettle; the amino acid solution feeding pipe is connected into the reaction kettle; the liquid caustic soda feeding pipe is connected into the reaction kettle; one end of the amino acid surface active product discharging pipe is connected into the bottom of the reaction kettle, and a reaction circulating pump is arranged on the amino acid surface active product discharging pipe; one end of the circulating pipe is connected to the amino acid surface active product discharging pipe through a three-way valve, the other end of the circulating pipe is connected into the reaction kettle and is tangent to the inner circumferential surface of the reaction kettle, a mixer and a heat exchanger are arranged on the circulating pipe, and an acyl chloride feeding pipe is connected to the circulating pipe located at the inlet end of the mixer. The high-efficiency amino acid surfactant circular reaction device provided by the utility model can effectively reduce side reactions such as acyl chloride hydrolysis and the like, improve the mass transfer efficiency, improve the conversion rate of materials and reduce the content of impurities in a product, so that the product quality is improved.

Description

Technical Field

[0001] The utility model relates to the technical field of surfactants, in particular to a high-efficiency amino acid surfactant circulation reaction device. Background Technique

[0002] With people paying more and more attention to the safety and mildness of various products and the improvement of environmental protection requirements, the development and use of high-quality environmentally friendly surfactants have been increasingly emphasized by countries around the world. Amino acid surfactants have good wetting properties, foaming properties, antibacterial properties, corrosion resistance, antistatic ability, etc., are almost non-toxic and harmless, and are mild to the skin. Their degradation products are amino acids and fatty acids, which have almost no impact on the environment, and also have the advantage of good compatibility with other various surfactants. Therefore, amino acid surfactants are widely used in application fields such as cosmetics (facial cleanser, body wash, shampoo, facial mask, etc.), detergents, and medical and health.

[0003] Currently, the amino acid surfactants on the market are mainly the following categories: sarcosine type, glycine type, glutamate type, alanine type, naphthylamine acid, proline, taurine, N-methyl taurine type, etc. It should be noted that currently, there are mainly two synthesis processes for amino acid surfactants in industry: the direct method and the indirect method. The direct method is the direct synthesis method from fatty acid raw materials. This method has low conversion rate, long reaction time, harsh reaction conditions, high equipment requirements, and high energy consumption, and has not been popularized in industrial production. The indirect method is the Schotten-Baumann condensation method in which acyl chloride replaces fatty acid to react with amino acid in an alkaline solution. It is the most widely used synthesis method in laboratories or industries. Acyl chloride and liquid alkali are both added from the upper part of the reactor, which has the advantages of relatively low equipment requirements, low price and easy availability of raw materials, mild reaction conditions, and easy treatment of by-products, and is deeply studying how to reduce acyl chloride hydrolysis and simplify product post-treatment. The main reaction equation of this method is:

[0004] Condensation reaction: HOOCCHR2NH2 + R1COCl → NaOOCCHR2NHCOR1. During the condensation reaction process, the most likely side reaction is the hydrolysis reaction of acyl chloride: Acyl chloride hydrolysis: R1COCl + 2NaOH → R1COONa + NaCl + H2O;

[0005] If acyl chloride undergoes hydrolysis, fatty acids or fatty acid salts will be generated, and this impurity is difficult to remove, which will affect the product quality. Therefore, reducing and inhibiting acyl chloride hydrolysis and improving the mass transfer efficiency and conversion rate of the condensation reaction are the keys to obtaining high-quality amino acid surfactants. Content of the Utility Model

[0006] The technical problem to be solved by the present utility model is to provide an efficient cyclic reaction device for amino acid surfactants in view of the deficiencies of the prior art, which can effectively reduce the occurrence of side reactions such as acyl chloride hydrolysis, improve the reaction mass transfer efficiency and conversion rate, and thus reduce the impurity content in the efficient cyclic reaction device for amino acid surfactants.

[0007] The technical problem to be solved by the present utility model is achieved through the following technical solutions. An efficient cyclic reaction device for amino acid surfactants includes a reaction kettle, which has:

[0008] A water injection pipe, which is connected to the inside of the reaction kettle;

[0009] An amino acid solution feeding pipe, which is connected to the inside of the reaction kettle;

[0010] A liquid caustic feeding pipe, which is connected to the inside of the reaction kettle;

[0011] An amino acid surfactant product discharging pipe, one end of which is connected to the bottom inside of the reaction kettle, and a reaction circulation pump is arranged thereon;

[0012] A circulation pipe, one end of the circulation pipe is connected to the amino acid surfactant product discharging pipe through a three-way valve, and the other end is connected to the inside of the reaction kettle and is tangent to the inner peripheral surface of the reaction kettle. A mixer and a heat exchanger are sequentially arranged on the circulation pipe in the fluid transportation direction. An acyl chloride feeding pipe is connected to the circulation pipe at the inlet end of the mixer.

[0013] The technical problem to be solved by the present utility model can also be achieved through the following technical solutions. In the above-mentioned efficient cyclic reaction device for amino acid surfactants, a bent pipe extending into the circulation pipe is arranged at the outlet end of the acyl chloride feeding pipe. The distance between the axis of the bent pipe and the axis of the circulation pipe is 2 / 3 of the radius of the circulation pipe, and the bent pipe is arranged towards the fluid flow direction in the circulation pipe.

[0014] The technical problem to be solved by the present utility model can also be achieved through the following technical solutions. In the above-mentioned efficient cyclic reaction device for amino acid surfactants, the outlet end of the liquid caustic feeding pipe and the outlet end of the circulation pipe are symmetrically arranged on both sides of the reaction kettle. The distances from the outlet ends of the liquid caustic feeding pipe and the circulation pipe to the center of the reaction kettle are both 2 / 3 of the radius of the reaction kettle.

[0015] The technical problem to be solved by the present utility model can also be achieved through the following technical solutions. In the above-mentioned efficient cyclic reaction device for amino acid surfactants, installation holes for the water injection pipe, the amino acid solution feeding pipe and the liquid caustic feeding pipe to extend into are reserved on the outer peripheral surface of the top of the reaction kettle, and the installation holes are equidistantly arranged from the outside to the inside on the top of the reaction kettle.

[0016] The technical problem to be solved by the utility model can also be achieved by the following technical scheme. In the above-mentioned high-efficiency amino acid surfactant circulating reaction device, a stirring mechanism is arranged in the reactor, and the stirring mechanism includes a variable frequency motor installed on the top of the reactor, and a stirring shaft extending into the reactor is transmission-connected to the power output end of the variable frequency motor, and stirring blades are fixedly provided on the bottom and the middle outer peripheral surface of the stirring shaft.

[0017] The technical problem to be solved by the utility model can also be achieved through the following technical scheme. In the above-mentioned high-efficiency amino acid surfactant circulating reaction device, the heat exchanger is a shell-and-tube heat exchanger with circulating inlet and outlet water.

[0018] The technical problem to be solved by the utility model can also be achieved by the following technical scheme: the above-mentioned high-efficiency amino acid surfactant circulation reaction device is provided with a steam heating jacket on the outer peripheral surface of the reactor.

[0019] The technical problem to be solved by the utility model can also be achieved by the following technical scheme: in the above-mentioned high-efficiency amino acid surfactant circulation reaction device, a remote liquid level meter is arranged in the reactor.

[0020] The technical problem to be solved by the utility model can also be achieved by the following technical scheme. In the above-mentioned high-efficiency amino acid surfactant circulation reaction device, the outlet end of the circulation pipe is divided into three pipes, namely, upper, middle and lower pipes. A control valve is installed on each pipe. The remote liquid level gauge is interlocked with the control valve. When the liquid level reaches 30%, the control valve on the bottom pipe is automatically opened. When the liquid level reaches 50%, the control valve on the middle pipe is automatically opened. When the liquid level reaches 70%, the control valve on the top pipe is opened.

[0021] Compared with the prior art, the beneficial technical effects of the utility model are:

[0022] (1) The outlet end of the liquid alkali feeding pipe and the outlet end of the circulation pipe are symmetrically arranged on both sides of the reactor, so that the acyl chloride can directly contact with the amino acid in the reactor when it is added to the reactor, avoiding the possibility of side reactions such as acyl chloride hydrolysis caused by direct contact between the acyl chloride and the liquid alkali, and ensuring that the acyl chloride can selectively and preferentially react with the amino acid in the system to undergo condensation reaction; in addition, the outlet end of the circulation pipe is tangent to the inner circumference of the reactor, which reduces the influence of the foam generated by the frontal impact between the materials on the reaction rate of the amino acid surfactant to a certain extent;

[0023] (2) The distance between the outlet end of the liquid caustic soda feeding pipe and the outlet end of the circulation pipe and the center of the reactor is 2 / 3 of the reactor radius, which makes the material linear velocity at this position the maximum, enabling the condensation reaction to be completed quickly, thereby significantly improving the mass transfer efficiency and conversion rate of the reaction and reducing the impurity content in the product;

[0024] (3) The outlet of the circulation pipe system is cleverly designed, divided into three pipes: upper, middle and lower. Each pipe is equipped with a precision control valve. The system is intelligently interlocked with the remote level gauge to ensure automated and efficient operation. When the liquid level reaches 30%, the system automatically opens the control valve on the bottom pipe to start the circulation and ensure that the circulation can be carried out below the liquid surface when the liquid level is low during the initial feeding. As the liquid level rises, when it reaches 50%, the control valve on the middle pipe automatically opens to further enhance the mixing effect. When the liquid level continues to rise to 70%, the control valve on the top pipe also automatically opens. This design can flexibly adapt to the mixing needs at different liquid level heights, greatly improving the practicality and efficiency of the system. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 This is a schematic diagram of the main structure of the utility model;

[0026] Figure 2 This is a partial structural schematic diagram of the utility model in which the acyl chloride feeding pipe is located in the circulation pipe.

[0027] Reference numerals:

[0028] 1. Reactor; 2. Stirring shaft; 3. Stirring blades; 4. Water injection pipe; 5. Amino acid solution feeding pipe; 6. Liquid alkali feeding pipe; 7. Amino acid surfactant product discharge pipe; 8. Circulation pipe; 9. Mixer; 10. Heat exchanger; 11. Acid chloride feeding pipe; 12. Bend pipe; 13. Steam heating jacket; 14. Remote level meter. DETAILED DESCRIPTION

[0029] The specific technical solutions of the present invention are further described below with reference to the accompanying drawings, so as to facilitate further understanding of the present invention by those skilled in the art, and do not constitute any limitation to the rights thereof.

[0030] Example 1, reference Figure 1-2 A high-efficiency amino acid surfactant circulation reaction device comprises a reactor 1, which is in the form of a roughly spherical reactor structure. A stirring mechanism is arranged in the reactor 1, and the stirring mechanism comprises a variable frequency motor installed on the top of the reactor 1. The model and specification of the variable frequency motor can be selected according to the use requirements. A stirring shaft 2 extending into the reactor 1 is connected to the power output end of the variable frequency motor in a transmission manner, and stirring blades 3 are fixedly arranged on the bottom and the middle outer peripheral surface of the stirring shaft 2. The reaction materials in the reactor 1 are fully mixed by the stirring mechanism, which helps to improve the reaction rate. By adjusting the parameters of the frequency converter to adapt to the stirring speed required under different working conditions such as reaction, maturation and defoaming, the generation of foam can be effectively reduced, and the mass transfer and heat transfer efficiency can be improved. It has:

[0031] The water injection pipe 4 is connected to the inside of the reactor 1;

[0032] The amino acid solution feeding pipe 5 is connected to the inside of the reactor 1;

[0033] The liquid caustic soda feeding pipe 6 is connected to the inside of the reactor 1;

[0034] The amino acid surfactant product discharging pipe 7 has one end connected to the bottom inside of the reactor 1, and a reaction circulation pump is arranged thereon. The reaction circulation pump is also configured with a variable frequency motor;

[0035] The circulation pipe 8 has its outlet end symmetrically placed below the liquid level of the reactor 1, which can not only reduce the foam generated by the interaction between the amino acid surfactant in the circulating material and air, but also enable the reaction materials to quickly contact each other, thereby strengthening the mass transfer effect and reducing the occurrence of side reactions;

[0036] One end of the circulation pipe 8 is connected to the amino acid surfactant product discharging pipe 7 through a three-way valve, and the other end is connected to the inside of the reactor 1 and is tangent to the inner peripheral surface of the reactor 1, which can reduce the influence of the foam generated by the frontal impact between the materials on the amino acid surfactant on the reaction rate to a certain extent. A mixer 9 and a heat exchanger 10 are sequentially arranged on the circulation pipe 8 in the fluid transportation direction. The heat exchanger 10 is a shell-and-tube heat exchanger with circulating in-and-out water. A chloride acyl feeding pipe 11 is connected to the circulation pipe 8 at the inlet end of the mixer 9. A bent pipe 12 extending into the circulation pipe 8 is arranged at the outlet end of the chloride acyl feeding pipe 11. The distance between the axis of the bent pipe 12 and the axis of the circulation pipe 8 is 2 / 3 of the radius of the circulation pipe 8, and the bent pipe 12 is arranged towards the fluid flow direction in the circulation pipe 8. The outlet ends of the liquid caustic soda feeding pipe 6 and the circulation pipe 8 are symmetrically arranged on both sides of the reactor 1, which enables the chloride acyl to directly contact the amino acid in the reactor 1 when being added to the reactor 1, avoiding the probability of side reactions such as the hydrolysis of the chloride acyl due to the direct contact between the chloride acyl and the liquid caustic soda, and ensuring that the chloride acyl can selectively and preferentially undergo a condensation reaction with the amino acid in the system;

[0037] The distances from the outlet ends of the liquid caustic soda feeding pipe 6 and the circulation pipe 8 to the center of the reactor 1 are both 2 / 3 of the radius of the reactor 1, which makes the linear velocity of the materials at this position the largest, enabling the condensation reaction to be completed quickly, thereby significantly improving the mass transfer efficiency and conversion rate of the reaction and reducing the impurity content in the product;

[0038] Installation holes for the water injection pipe 4, the amino acid solution feeding pipe 5 and the liquid caustic soda feeding pipe 6 to extend are reserved on the outer peripheral surface of the top of the reactor 1, and the installation holes are equidistantly arranged on the top of the reactor 1 from the outside to the inside;

[0039] A steam heating jacket 13 is arranged on the outer peripheral surface of the reactor 1, which is used to provide heat for the ripening and defoaming of the amino acid surfactant product in the later stage;

[0040] A remote transmission liquid level gauge 14 is provided inside the reaction kettle, and the height of the liquid level inside the reaction kettle 1 can be learned through the remote transmission liquid level gauge 14.

[0041] In Example 1, the outlet end of the circulation pipe can be divided into three upper, middle and lower pipes, and control valves are installed on each pipe. The remote transmission liquid level gauge is interlocked with the control valve. When the liquid level reaches 30%, the control valve on the lowermost pipe is automatically opened. When the liquid level reaches 50%, the control valve on the middle pipe is automatically opened. When the liquid level reaches 70%, the control valve on the uppermost pipe is opened.

[0042] The outlet end of the circulation pipe system is ingeniously designed and divided into three upper, middle and lower pipelines, and each pipeline is equipped with a precision control valve. The system is intelligently interlocked with the remote transmission liquid level gauge to ensure automatic and efficient operation. When the liquid level reaches 30%, the control valve on the lowermost pipeline will be automatically opened to start the circulation and ensure that the circulation can also be carried out below the liquid level when the liquid level is low during the initial feeding. As the liquid level rises, when it reaches 50%, the control valve on the middle pipeline is automatically opened to further enhance the mixing effect. When the liquid level continues to rise to 70%, the control valve on the uppermost pipeline is also automatically opened. Such a design can flexibly adapt to the mixing requirements at different liquid level heights, greatly improving the practicability and efficiency of the system.

[0043] The circulation reaction process of the high-efficiency amino acid surfactant circulation reaction device is as follows:

[0044] S1. Put a quantitative amino acid solution and water into the reaction kettle 1 respectively, and then turn on the stirring mechanism of the reaction kettle 1 to mix the materials evenly;

[0045] S2. Pass circulating cooling water into the reaction circulation heat exchanger 10, and then start the reaction circulation pump;

[0046] S3. Dropwise add acyl chloride through the acyl chloride feeding pipe 11, and control the dropping rate of acyl chloride and the temperature of the materials during the dropping process;

[0047] S4. Dropwise add liquid alkali through the liquid alkali feeding pipe 6, and control the pH of the materials during the dropping process;

[0048] S5. After the dropping of acyl chloride and liquid alkali is completed, continue to stir to make the materials react fully;

[0049] S6. Open the steam heating jacket 13 of the reaction kettle 1 to heat the heat source, raise the temperature of the materials for ripening, then take samples to analyze the solid content and pH, and add water to adjust to qualified solid content and pH;

[0050] S7. Continue to raise the temperature of the materials in the reaction kettle 1, and obtain an amino acid surfactant product after defoaming;

[0051] Further, in step S1, the amino acid can be one of sodium sarcosinate, sodium glycinate, sodium glutamate, sodium alaninate, sodium N-methyl taurate, potassium glycinate, potassium glutamate, sodium naphthylamine sulfonate, sodium prolinate, sodium taurine, sodium N-methyl taurate, and the stirring time is controlled within 10 to 30 min;

[0052] Further, in step S2, the temperature of the circulating cooling water is controlled at 0 to 30°C (the temperature of taurine-based is controlled at 30 to 60°C);

[0053] Further, in step S3, the acyl chloride can be one of lauroyl chloride and coconut oil acyl chloride, the dropping rate of the acyl chloride is controlled at 60 to 360 kg / h, and the temperature of the material in reactor 1 is controlled at 10 to 35°C (the temperature of taurine-based is controlled at 30 to 70°C);

[0054] Further, in step S4, the liquid alkali can be one of sodium hydroxide solution and potassium hydroxide solution, and the pH of the material in reactor 1 is controlled at 9.0 to 11.5;

[0055] Further, in step S5, the stirring time in reactor 1 is controlled at 20 to 30 min;

[0056] Further, in step S6, the jacket heating heat source of reactor 1 can be one of steam and hot water, the temperature of the material in reactor 1 is raised to 30 to 80°C, and the aging time is controlled at 60 to 90 min;

[0057] Further, in step S7, the temperature of the material in reactor 1 is raised to 80 to 85°C, and the defoaming time is controlled at 60 to 120 min.

Claims

1. An efficient cyclic reaction device for amino acid surfactants, characterized in that: It includes a reaction kettle having: A water injection pipe connected to the reactor; An amino acid solution feeding pipe connected to the reactor; A liquid caustic soda feeding pipe connected to the reactor; An amino acid surfactant product discharge pipe, one end of which is connected to the bottom of the reactor, and a reaction circulation pump is arranged on it; A circulation pipe, one end of which is connected to the discharge pipe of the amino acid surfactant product through a three-way valve, and the other end is connected to the reactor and is tangent to the inner circumference of the reactor. A mixer and a heat exchanger are arranged in sequence on the circulation pipe according to the fluid conveying direction, and an acyl chloride feeding pipe is connected to the circulation pipe at the inlet end of the mixer.

2. The high-efficiency amino acid surfactant cyclic reaction device according to claim 1, characterized in that: The outlet end of the acyl chloride feeding pipe is provided with a bend extending into the circulation pipe, the distance between the axis of the bend and the axis of the circulation pipe is 2 / 3 of the radius of the circulation pipe, and the bend is arranged toward the flow direction of the fluid in the circulation pipe.

3. An efficient amino acid surfactant cyclic reaction device according to claim 1, characterized in that: The outlet ends of the liquid alkali feeding pipe and the circulating pipe are symmetrically placed on both sides of the reactor, and the distances from the outlet ends of the liquid alkali feeding pipe and the circulating pipe to the center of the reactor are both 2 / 3 of the radius of the reactor.

4. An efficient amino acid surfactant cyclic reaction device according to claim 1, characterized in that: The top outer peripheral surface of the reactor is reserved with installation holes for water injection pipes, amino acid solution feeding pipes and liquid alkali feeding pipes to extend into, and the installation holes are arranged equidistantly on the top of the reactor from outside to inside.

5. An efficient amino acid surfactant cyclic reaction device according to claim 1, characterized in that: The reactor is provided with a stirring mechanism, which includes a variable frequency motor installed on the top of the reactor, a stirring shaft extending into the reactor is transmission-connected to the power output end of the variable frequency motor, and stirring blades are fixed on the bottom and middle outer peripheral surface of the stirring shaft.

6. An efficient amino acid surfactant cyclic reaction device according to claim 1, characterized in that: The heat exchanger is a shell-and-tube heat exchanger with circulating water inlet and outlet.

7. An efficient amino acid surfactant cyclic reaction device according to claim 1, characterized in that: A steam heating jacket is arranged on the outer peripheral surface of the reaction kettle.

8. An efficient amino acid surfactant cyclic reaction device according to claim 1, characterized in that: A remote liquid level gauge is arranged in the reactor.

9. An efficient amino acid surfactant cyclic reaction device according to claim 8, characterized in that: The outlet end of the circulation pipe is divided into three pipes: upper, middle and lower. A control valve is installed on each pipe. The remote liquid level gauge is interlocked with the control valve. When the liquid level reaches 30%, the control valve on the bottom pipe is automatically opened. When the liquid level reaches 50%, the control valve on the middle pipe is automatically opened. When the liquid level reaches 70%, the control valve on the top pipe is opened.

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