Method for producing vegetable protein fiber and silk by using vegetable protein

Abstract

The invention relates to the technical field of protein fibers, and provides a method for producing plant protein fibers by using plant proteins, which comprises the following steps: S1, dissolving the plant proteins to obtain a plant protein solution; s2, mixing the vegetable protein solution with an active agent to obtain a mixture; s3, after the mixture and a polyvinyl alcohol solution are mixed, a cross-linking agent and an auxiliary A are sequentially added for mixing, a spinning solution is obtained, and plant protein fibers are obtained through spinning; the auxiliary agent A is prepared from the following components in parts by weight: 10 to 18 parts of flame retardant, 0.2 to 0.4 part of pH (Potential of Hydrogen) regulator and 0.3 to 0.8 part of tackifier; the flame retardant comprises dipropyl aluminum hypophosphite and titanium dioxide in a mass ratio of (1: 19)-(19: 1). By means of the technical scheme, the problem that in the prior art, the flame retardance of vegetable protein fibers is poor is solved.

Description

Technical Field

[0001] The present invention relates to the technical field of plant protein fibers, and in particular to a method for producing plant protein fibers and silk by utilizing plant protein. Background Art

[0002] Plant protein fiber is mainly composed of protein, and its molecular structure contains a large amount of carbon, hydrogen, oxygen and other elements. After it is made into fabric, these elements will generate heat when burned, thereby accelerating the burning of the fiber. In addition, the molecular structure of plant protein fiber lacks flame retardant elements, such as nitrogen, phosphorus, chlorine, etc., which makes its flame retardant performance poor, which not only limits its application in some special fields, but also limits the research and development direction of plant protein fiber.

[0003] Therefore, it is urgent to solve the problem of poor flame retardancy of current plant protein fibers, increase the application demand of plant protein fibers in specific fields, and promote the sustainable development of plant protein fibers. Summary of the invention

[0004] The invention provides a method for producing plant protein fiber and silk by utilizing plant protein, which solves the problem of poor flame retardancy of plant protein fiber in the related art.

[0005] The technical solution of the present invention is as follows: The present invention provides a method for producing plant protein fiber using plant protein, comprising the following steps: S1, dissolving the plant protein to obtain a plant protein solution; S2, mixing the plant protein solution and the active agent to obtain a mixture; S3, after mixing the mixture and the polyvinyl alcohol solution, adding a cross-linking agent and an auxiliary agent A in sequence to mix, to obtain a spinning solution, and spinning to obtain a plant protein fiber; The auxiliary agent A comprises the following components in parts by weight: 10-18 parts of flame retardant, 0.2-0.4 parts of pH adjuster, and 0.3-0.8 parts of tackifier; The flame retardant comprises dipropyl aluminum hypophosphite and titanium dioxide in a mass ratio of 1:19 to 19:1.

[0006] As a further technical solution, the cross-linking agent includes one or more of formaldehyde, glutaraldehyde, and dibenzoyl peroxide; The mass ratio of the cross-linking agent to the plant protein is 1-2:10.

[0007] As a further technical solution, the components of the active agent include sodium phosphate, sodium hydroxide, and acetamide in a mass ratio of 1:0.1:1-3; The mass ratio of the active agent to the plant protein is 0.1-0.2:3.

[0008] As a further technical solution, the flame retardant comprises components of dipropyl aluminum hypophosphite and titanium dioxide in a mass ratio of 3:2 to 5:1.

[0009] In the present invention, dipropyl aluminum hypophosphite and titanium dioxide are added in a mass ratio of 3:2 to 5:1 as components of the flame retardant to the plant protein fiber for synergistic enhancement, thereby further improving the flame retardancy of the plant protein fiber.

[0010] As a further technical solution, the titanium dioxide is brominated polystyrene modified titanium dioxide.

[0011] As a further technical solution, the flame retardant is a 2-hydroxycyclohexanecarboxylic acid modified flame retardant.

[0012] As a further technical solution, the preparation method of the flame retardant includes the following steps: dissolving brominated polystyrene and mixing it with titanium dioxide, drying it to obtain brominated polystyrene modified titanium dioxide, mixing a dissolved solution of 2-hydroxycyclohexanecarboxylic acid with the brominated polystyrene modified titanium dioxide, and drying it to obtain a flame retardant.

[0013] As a further technical solution, the mass ratio of the brominated polystyrene, 2-hydroxycyclohexanecarboxylic acid and the titanium dioxide is 1:1:12-16.

[0014] In the present invention, brominated polystyrene is used to modify titanium dioxide, and then 2-hydroxycyclohexanecarboxylic acid is used to modify the brominated polystyrene modified titanium dioxide and dipropyl aluminum hypophosphite, thereby further improving the flame retardancy and strength of the plant protein fiber.

[0015] As a further technical solution, the pH regulator is an inorganic acid; the viscosity enhancer is one or both of hydroxymethyl cellulose and starch; and the plant protein includes one or both of soy protein and corn protein.

[0016] The invention also proposes the use of the plant protein fiber prepared by the method as raw material for preparing silk.

[0017] The working principle and beneficial effects of the present invention are: In the present invention, dipropyl aluminum hypophosphite and titanium dioxide are added to the plant protein fiber as components of the flame retardant for synergistic enhancement. After the plant protein fiber is made with other components, the flame retardancy of the plant protein fiber is significantly improved. DETAILED DESCRIPTION

[0018] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0019] In the following examples and comparative examples, the weight average molecular weight of brominated polystyrene is 60,000.

[0020] Example 1 A method for producing plant protein fiber using plant protein comprises the following steps: S1, dissolving corn protein to obtain a plant protein solution; S2, mixing the plant protein solution and the active agent to obtain a mixture; S3, mixing the mixture and a polyvinyl alcohol solution with a mass fraction of 10% (the weight average molecular weight of the polyvinyl alcohol is 5000), adding glutaraldehyde and auxiliary agent A in sequence, mixing, to obtain a spinning solution, and spinning to obtain plant protein fibers; Additive A includes the following components in parts by weight: 15 parts of flame retardant, 0.3 parts of phosphoric acid, and 0.5 parts of starch; the mass ratio of glutaraldehyde to corn protein is 1:10; the components of the active agent include sodium phosphate, sodium hydroxide, and acetamide in a mass ratio of 1:0.1:2; the mass ratio of the active agent to corn protein is 0.1:3; the flame retardant is dipropyl aluminum hypophosphite and titanium dioxide in a mass ratio of 1:19.

[0021] Example 2 A method for producing plant protein fiber using plant protein comprises the following steps: S1, dissolving the soybean protein to obtain a vegetable protein solution; S2, mixing the plant protein solution and the active agent to obtain a mixture; S3, mixing the mixture and a polyvinyl alcohol solution with a mass fraction of 10% (the weight average molecular weight of the polyvinyl alcohol is 5000), adding glutaraldehyde and auxiliary agent A in sequence, mixing, to obtain a spinning solution, and spinning to obtain plant protein fibers; Additive A includes the following components in parts by weight: 18 parts of flame retardant, 0.4 parts of phosphoric acid, and 0.8 parts of starch; the mass ratio of glutaraldehyde to soy protein is 1:5; the components of the active agent include sodium phosphate, sodium hydroxide, and acetamide in a mass ratio of 1:0.1:1; the mass ratio of the active agent to soy protein is 0.2:3; the flame retardant is dipropyl aluminum hypophosphite and titanium dioxide in a mass ratio of 19:1.

[0022] Example 3 A method for producing plant protein fiber using plant protein comprises the following steps: S1, dissolving the soybean protein to obtain a vegetable protein solution; S2, mixing the plant protein solution and the active agent to obtain a mixture; S3, mixing the mixture and a polyvinyl alcohol solution with a mass fraction of 10% (the weight average molecular weight of the polyvinyl alcohol is 5000), adding glutaraldehyde and auxiliary agent A in sequence, mixing, to obtain a spinning solution, and spinning to obtain plant protein fibers; Additive A includes the following components in parts by weight: 10 parts of flame retardant, 0.2 parts of phosphoric acid, and 0.3 parts of starch; the mass ratio of glutaraldehyde to soy protein is 1:10; the components of the active agent include sodium phosphate, sodium hydroxide, and acetamide in a mass ratio of 1:0.1:3; the mass ratio of the active agent to soy protein is 0.1:3; the flame retardant is dipropyl aluminum hypophosphite and titanium dioxide in a mass ratio of 1:1.

[0023] Example 4 The only difference between this embodiment and embodiment 3 is that the flame retardant is dipropyl aluminum hypophosphite and titanium dioxide in a mass ratio of 6:1.

[0024] Example 5 The only difference between this embodiment and embodiment 3 is that the flame retardant is dipropyl aluminum hypophosphite and titanium dioxide in a mass ratio of 3:2.

[0025] Example 6 The only difference between this embodiment and embodiment 3 is that the flame retardant is dipropyl aluminum hypophosphite and titanium dioxide in a mass ratio of 5:1.

[0026] Example 7 The difference between this embodiment and embodiment 6 is that the flame retardant is dipropyl aluminum hypophosphite and brominated polystyrene modified titanium dioxide in a mass ratio of 5:1; The preparation method of brominated polystyrene modified titanium dioxide comprises the following steps: dissolving 1 g of brominated polystyrene in 40 g of DMF, adding 12 g of titanium dioxide, mixing, and drying to obtain brominated polystyrene modified titanium dioxide.

[0027] Example 8 The difference between this embodiment and embodiment 6 is that the flame retardant is dipropyl aluminum hypophosphite and brominated polystyrene modified titanium dioxide in a mass ratio of 5:1; The preparation method of brominated polystyrene modified titanium dioxide comprises the following steps: dissolving 1g of 2-hydroxycyclohexanecarboxylic acid in 40g of 70% by volume ethanol, adding 12g of titanium dioxide for mixing, and drying to obtain brominated polystyrene modified titanium dioxide.

[0028] Example 9 The difference between this embodiment and embodiment 6 is that the flame retardant is dipropyl aluminum hypophosphite and brominated polystyrene modified titanium dioxide in a mass ratio of 5:1; The preparation method of the flame retardant comprises the following steps: dissolving 1g of brominated polystyrene in 40g of DMF, adding 12g of titanium dioxide to mix, and drying to obtain brominated polystyrene modified titanium dioxide; dissolving 1g of 2-hydroxycyclohexanecarboxylic acid in 40g of 70% by volume ethanol, adding brominated polystyrene modified titanium dioxide and dipropyl aluminum hypophosphite to mix, and drying to obtain brominated polystyrene modified titanium dioxide.

[0029] Example 10 The difference between this embodiment and embodiment 6 is that the flame retardant is dipropyl aluminum hypophosphite and brominated polystyrene modified titanium dioxide in a mass ratio of 5:1; The preparation method of the flame retardant comprises the following steps: dissolving 1g of brominated polystyrene in 50g of DMF, adding 16g of titanium dioxide to mix, and drying to obtain brominated polystyrene modified titanium dioxide; dissolving 1g of 2-hydroxycyclohexanecarboxylic acid in 50g of 70% by volume ethanol, adding brominated polystyrene modified titanium dioxide and dipropyl aluminum hypophosphite to mix, and drying to obtain brominated polystyrene modified titanium dioxide.

[0030] Comparative Example 1 The only difference between this comparative example and Example 3 is that the flame retardant is dipropyl aluminum hypophosphite.

[0031] Comparative Example 2 The only difference between this comparative example and Example 3 is that the flame retardant is titanium dioxide.

[0032] The performance tests were performed on the plant protein fibers prepared in Examples 1 to 10 and Comparative Examples 1 to 2 respectively: Flame retardancy: tested in accordance with standard FZ / T 50016-2023 "Test method for combustion performance of chemical fibers - oxygen index method"; Strength: Breaking strength test is carried out according to standard GB / T 14337-2022 "Test method for tensile properties of chemical staple fibers"; The results are shown in Tables 1~2 below.

[0033] Table 1 Flame retardant performance test results

[0034] By comparing the data of Examples 1 to 10 and Comparative Examples 1 to 2, it is found that compared with Comparative Examples 1 to 2, the oxygen index of the plant protein fiber obtained in Examples 1 to 10 is higher, indicating that the addition of dipropyl aluminum hypophosphite and titanium dioxide as components of the flame retardant in the plant protein fiber synergistically enhances the flame retardancy of the plant protein fiber.

[0035] By comparing the data of Examples 3 to 6, it was found that compared with Examples 3 to 4, the oxygen index of the plant protein fiber obtained in Examples 5 to 6 was higher, indicating that the addition of dipropyl aluminum hypophosphite and titanium dioxide in a mass ratio of 3:2 to 5:1 as components of the flame retardant in the plant protein fiber synergistically enhanced the flame retardancy of the plant protein fiber.

[0036] By comparing the data of Examples 6 to 10, it is found that compared with Examples 6 to 8, the oxygen index of the plant protein fiber obtained in Examples 9 to 10 is higher, indicating that after the brominated polystyrene is used to modify the titanium dioxide, and then the brominated polystyrene-modified titanium dioxide and dipropyl aluminum hypophosphite are modified by a modifier, the flame retardancy of the plant protein fiber is further improved.

[0037] Table 2 Strength test results

[0038] By comparing the data of Examples 7 to 10, it is found that compared with Example 7, the dry and wet breaking strengths of the plant protein fibers obtained in Examples 8 to 10 are higher, indicating that the use of brominated polystyrene to modify titanium dioxide or the use of 2-hydroxycyclohexanecarboxylic acid to modify the flame retardant further improves the strength of the plant protein fiber; compared with Examples 8 to 9, the dry and wet breaking strengths of the plant protein fibers obtained in Example 10 are higher, indicating that the use of brominated polystyrene to modify titanium dioxide and the use of 2-hydroxycyclohexanecarboxylic acid to modify the flame retardant further improve the strength of the plant protein fiber.

[0039] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for producing plant protein fiber using plant protein, characterized in that: The following steps are involved: S1, dissolving the plant protein to obtain a plant protein solution; S2, mixing the plant protein solution and the active agent to obtain a mixture; S3, after mixing the mixture and the polyvinyl alcohol solution, adding a cross-linking agent and an auxiliary agent A in sequence to mix, to obtain a spinning solution, and spinning to obtain a plant protein fiber; The auxiliary agent A comprises the following components in parts by weight: 10-18 parts of flame retardant, 0.2-0.4 parts of pH adjuster, and 0.3-0.8 parts of tackifier; The flame retardant comprises dipropyl aluminum hypophosphite and titanium dioxide in a mass ratio of 1:19 to 19:

1.

2. The method for producing plant protein fiber using plant protein according to claim 1, characterized in that: The cross-linking agent includes one or more of formaldehyde, glutaraldehyde, and dibenzoyl peroxide; The mass ratio of the cross-linking agent to the plant protein is 1-2:

10.

3. The method for producing plant protein fiber using plant protein according to claim 1, characterized in that: The components of the active agent include sodium phosphate, sodium hydroxide and acetamide in a mass ratio of 1:0.1:1-3; The mass ratio of the active agent to the plant protein is 0.1-0.2:

3.

4. The method for producing plant protein fiber using plant protein according to claim 1, characterized in that: The flame retardant comprises dipropyl aluminum hypophosphite and titanium dioxide in a mass ratio of 3:2 to 5:

1.

5. The method for producing plant protein fiber using plant protein according to claim 1, characterized in that: The titanium dioxide is brominated polystyrene modified titanium dioxide.

6. The method for producing plant protein fiber using plant protein according to claim 5, characterized in that: The flame retardant is a 2-hydroxycyclohexanecarboxylic acid modified flame retardant.

7. The method for producing plant protein fiber using plant protein according to claim 6, characterized in that: The preparation method of the flame retardant comprises the following steps: dissolving brominated polystyrene, mixing the mixture with titanium dioxide, and drying to obtain brominated polystyrene modified titanium dioxide; mixing a solution of 2-hydroxycyclohexanecarboxylic acid with the brominated polystyrene modified titanium dioxide and dipropyl aluminum hypophosphite, and drying to obtain the flame retardant.

8. The method for producing plant protein fiber using plant protein according to claim 7, characterized in that: The mass ratio of the brominated polystyrene, 2-hydroxycyclohexanecarboxylic acid and the titanium dioxide is 1:1:12-16.

9. The method for producing plant protein fiber using plant protein according to claim 1, characterized in that: The pH regulator is an inorganic acid; the viscosity enhancer is one or both of hydroxymethyl cellulose and starch; and the plant protein includes one or both of soy protein and corn protein.

10. Use of the plant protein fiber obtained by the method according to any one of claims 1 to 9 as a raw material for silk preparation.

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