Preparation method of vulcanized modified wood flour reinforcing material

By blending the high-temperature pretreated wood powder with elemental sulfur, reacting at high temperature and desulfurization and drying, vulcanized modified wood powder reinforcement materials are prepared, which solves the pollution and agglomeration of traditional reinforcement materials, and achieves good rubber reinforcement effect and cost reduction.

CN119820675APending Publication Date: 2025-04-15QILU UNIVERSITY OF TECHNOLOGY (SHANDONG ACADEMY OF SCIENCES)
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Patent Information

Application Number
CN202510261773.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-06
Publication Date
2025-04-15

AI Technical Summary

Technical Problem

Traditional rubber reinforcement materials such as carbon black will produce a large amount of waste gas and pollution during the production process, and are prone to agglomeration, which increases the mixing time and energy consumption.

Method used

By blending the high-temperature pretreated wood powder with elemental sulfur, performing high-temperature reaction, it is desulfurized, washed with water and freeze-dried to obtain a vulcanized modified wood powder reinforcement material.

Benefits of technology

The prepared vulcanized modified wood powder reinforcement material has good reinforcement properties and good compatibility with the rubber matrix, which can improve the strength of the rubber and reduce production costs.

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Abstract

The invention discloses a preparation method of a vulcanization modified wood flour reinforcing material. The method comprises the following steps: firstly, drying wood flour, then carrying out high-temperature pretreatment, blending the wood flour subjected to high-temperature pretreatment with elemental sulfur, carrying out high-temperature reaction, carrying out solvent desulfurization on the product, washing with water, and freeze-drying to obtain the product vulcanized wood flour. The sulfur modified wood powder has a good reinforcing effect, is wide in source and relatively low in cost, can reduce the production cost of rubber products while ensuring the reinforcing effect of rubber, and has a wide application prospect.
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Description

Technical Field

[0001] The invention relates to the field of preparation of rubber reinforcing agents, in particular to a method for preparing a vulcanized modified wood powder reinforcing material, and belongs to the technical field of functional polymer materials. Background Art

[0002] As a key material in tire manufacturing, people's demand for rubber is increasing. A large number of tires for automobiles, airplanes and other vehicles produced worldwide every year rely on rubber; in addition, rubber is also used to make medical rubber gloves, sealing materials, etc. However, the development of rubber also has disadvantages. Traditional reinforcing materials such as carbon black will produce a large amount of waste gas such as carbon dioxide, carbon monoxide and sulfide during the production process. Improper waste gas treatment will pollute the atmospheric environment. In addition, carbon black is prone to agglomeration, which increases mixing time and energy consumption. In recent years, people have been trying to find reinforcing materials with good reinforcement properties and low prices to replace carbon black.

[0003] Sulfur is a naturally occurring element with a long history of use. Sulfur is mainly derived from natural sulfur ore. In areas with frequent volcanic activity, underground sulfur is brought to the surface by volcanic eruptions to form sulfur ore. These ores can be mined and refined to obtain sulfur. In addition, during the refining process, sulfur compounds in crude oil are decomposed, resulting in sulfur as a by-product. Sulfur is a key raw material for the manufacture of sulfuric acid, which is one of the most important products in the chemical industry. It can be used to make phosphate fertilizers such as superphosphate and to treat ores. Sulfur is a vulcanizing agent in the vulcanization process of rubber. Sulfur reacts with rubber molecules to form a cross-linked structure, which significantly improves the physical properties of rubber, such as elasticity, wear resistance, and aging resistance, so that a variety of high-quality rubber products, such as tires and hoses, can be produced.

[0004] Wood powder is a powdery substance processed from wood. Wood powder is a natural fibrous material whose main components are cellulose, hemicellulose and lignin. It can play a supporting role similar to that of a skeleton in the rubber matrix. The functional groups such as hydroxyl groups on the surface of wood powder can interact physically or chemically with the active groups on the rubber molecular chain to form chemical bonds or strong hydrogen bonds. This interfacial interaction enhances the bonding force between wood powder and rubber, allowing wood powder to better play a reinforcing role in rubber and prevent wood powder from agglomerating in the rubber matrix or falling off from the rubber. Vulcanized wood powder as a rubber reinforcing agent can not only effectively utilize wood resources, but also reduce the cost of rubber production to a certain extent.

[0005] By utilizing the property of sulfur opening the ring at high temperature and the property of wood powder dehydration at high temperature to produce unsaturated bonds, sulfur and wood powder undergo addition reaction and the resulting sulfurized wood powder has good reinforcing properties and certain vulcanization properties. Summary of the invention

[0006] The object of the present invention is to provide a method for preparing a vulcanized modified wood powder reinforcing material. The preparation method is simple to operate, the process is controllable, the conditions are mild, and the cost is low. The prepared vulcanized modified wood powder reinforcing material has good reinforcing performance, good compatibility with a rubber matrix, uniform dispersion, can improve the strength of the rubber, and has broad application prospects.

[0007] In order to achieve the purpose of the present invention, the following technical solutions are provided:

[0008] A method for preparing a vulcanized modified wood powder reinforcement material, characterized by the following steps:

[0009] The wood powder pretreated at high temperature is mixed with elemental sulfur, reacted at high temperature, the product is desulfurized by solvent, washed with water, and freeze-dried to obtain the product sulfurized wood powder.

[0010] The mass ratio of wood powder to sulfur in the synthetic sulfurized wood powder is 1:0.2-2.

[0011] The wood powder pretreatment temperature is further described as 150°C to 250°C, and the time is 1 to 24 hours.

[0012] The reaction conditions are further described as temperature of 110-200° C. and time of 1-24 h.

[0013] Compared with the prior art, the present invention has the following beneficial effects:

[0014] Through the preparation method of the vulcanized modified wood powder reinforcing material of the present invention, the raw material cost of preparing the vulcanized modified wood powder reinforcing material is low and the source is wide. It can be used as a reinforcing agent in the rubber production process, is easy to promote and use, and has a wide application prospect. DETAILED DESCRIPTION

[0015] The present invention will be further described below by specific embodiments. The following examples are intended to illustrate the present invention rather than further limit the present invention. In addition, it should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms also fall within the scope limited by the appended claims of the application.

[0016] Embodiment 1:

[0017] Weigh 5.3g of wood powder and 3g of elemental sulfur, pre-treat the wood powder in a closed manner at 190°C, mix the treated wood powder with sulfur and place it in a hydrothermal reactor, then put it in an oven, adjust the oven temperature to 180°C, and react for 24 hours to allow the elemental sulfur to react with the treated wood powder to generate sulfurized wood powder. Then use toluene to remove sulfur from the product, and the product after sulfur removal is washed with water and cold-dried to obtain a sulfurized modified wood powder reinforcement material.

[0018] After the prepared vulcanized modified wood powder was blended with natural rubber and then subjected to steps such as mixing, it was found that the vulcanized modified wood powder had a good reinforcing effect on the rubber.

[0019] Embodiment 2:

[0020] Weigh 5.43g of wood powder and 3.13g of elemental sulfur, pre-treat the wood powder in a closed environment at 190°C, mix the treated wood powder with sulfur and place it in a hydrothermal reactor, then put it in an oven, adjust the oven temperature to 180°C, and react for 24 hours to allow the elemental sulfur to react with the treated wood powder to generate sulfurized wood powder. Then use toluene to remove sulfur from the product, and the product after sulfur removal is washed with water and cold-dried to obtain a sulfurized modified wood powder reinforcement material.

[0021] After the prepared vulcanized modified wood powder was blended with styrene-butadiene rubber and then subjected to steps such as mixing, it was found that the vulcanized modified wood powder had a good reinforcing effect on the rubber.

Claims

1. A method for preparing a vulcanized modified wood powder reinforcement material, characterized by the following steps: The wood powder pretreated at high temperature is mixed with elemental sulfur, reacted at high temperature, the product is desulfurized by solvent, washed with water, and freeze-dried to obtain the product sulfurized wood powder.

2. The method for preparing a vulcanized modified wood powder reinforcement material according to claim 1, characterized in that The mass ratio of wood powder to sulfur in synthetic sulfurized wood powder is 1:0.2-2.

3. The method for preparing a vulcanized modified wood powder reinforcement material as claimed in claim 1, wherein the pretreatment temperature of the wood powder is 150°C to 250°C and the pretreatment time is 1 to 24 hours.

4. The method for preparing a vulcanized modified wood powder reinforcement material according to claim 1, characterized in that The reaction conditions for synthesizing sulfurized wood powder are a temperature of 110°C to 200°C and a time of 1 to 24 hours.