Hydrofluoric acid protective clothing and method of making same

Abstract

The application relates to the technical field of chemical protection materials, and discloses a hydrofluoric acid protective garment and a preparation method thereof. The material of the protective garment comprises a 5-layer structure, the middle layer is a framework fabric, and modified natural rubber layers and modified EPDM (ethylene propylene diene monomer) rubber layers are sequentially arranged on the two sides of the framework fabric. The raw materials of the modified natural rubber comprise, by weight parts, natural rubber 100 parts, sulfur 3-4 parts, accelerator M 1-2 parts, accelerator DM 1-2 parts, zinc oxide 4-6 parts, stearic acid 1-2 parts, white carbon black 10-15 parts, calcium oxide 20-40 parts, chlorinated paraffin 5-15 parts, antimony trioxide 5-15 parts and antioxidant 4010NA 1-2 parts. The modified natural rubber and the modified EPDM rubber are used as main protection substances, and organic solvents are used as carriers, so that the hydrofluoric acid protective garment not only has long-acting protection capability for hydrofluoric acid, but also has the characteristics of high mechanical strength, heat aging resistance, flame resistance and low-temperature softness.

Description

Technical Field

[0001] This invention relates to the field of chemical protective materials technology, and more specifically to a hydrofluoric acid protective suit and its preparation method. Background Technology

[0002] In recent years, my country's fluorochemical industry has developed rapidly and has become an important part of the country's strategic emerging industries, covering fields such as fluorochemistry, fluorochemicals, fluorinated pharmaceuticals, pesticides and functional materials. Among them, anhydrous hydrofluoric acid is one of the most important basic raw materials in the fluorochemical industry. In 2019, my country's actual production of anhydrous hydrofluoric acid was about 1.508 million tons.

[0003] Hydrofluoric acid is a highly toxic chemical. Contact with it can cause skin irritation, such as initial redness and dryness. As the condition progresses, it can cause the skin to turn black or grayish-black. Later exposure can also allow fluoride ions to penetrate the skin and reach the deeper layers of the dermis, potentially leading to tissue necrosis. Therefore, the demand for hydrofluoric acid protective equipment is steadily increasing.

[0004] Currently, my country lacks a single standard for hydrofluoric acid protection. While ordinary chemical protective clothing offers good overall performance, its protection against hydrofluoric acid is poor, making it unsuitable for manual labor in the fluorination industry. In the chemical industry, particularly in fluorination, domestically produced PVC protective clothing offers approximately 1-2 hours of protection against 40% hydrofluoric acid. However, PVC protective clothing is prohibited for practical use abroad and is only permitted as training clothing. Imported protective clothing made from non-woven fabric and plastic film composite materials offers approximately 3-4 hours of protection against 40% hydrofluoric acid, but its poor physical and mechanical properties make it prone to tearing and loss of protective effectiveness due to abrasion.

[0005] Therefore, how to provide a hydrofluoric acid protective suit with high physical and mechanical strength, comfort, softness, and good protective performance, and its preparation method, is a problem that urgently needs to be solved by those skilled in the art. Summary of the Invention

[0006] In view of this, the present invention provides a hydrofluoric acid protective suit and a method for preparing the same.

[0007] To achieve the above objectives, the present invention adopts the following technical solution:

[0008] A hydrofluoric acid protective suit, the protective suit being made of a 5-layer structure, with a middle layer being a skeleton fabric, and modified natural rubber layer and modified EPDM rubber layer being sequentially arranged on both sides of the skeleton fabric.

[0009] Furthermore, the skeleton fabric is a polyester fabric.

[0010] Furthermore, the raw materials for the modified natural rubber, by weight, include: 100 parts natural rubber, 3-4 parts sulfur, 1-2 parts accelerator M, 1-2 parts accelerator DM, 4-6 parts zinc oxide, 1-2 parts stearic acid, 10-15 parts silica, 20-40 parts calcium oxide, 5-15 parts chlorinated paraffin, 5-15 parts antimony trioxide, and 1-2 parts antioxidant 4010NA.

[0011] Further, the raw materials for the modified EPDM rubber, by weight, include: 100 parts EPDM rubber, 1-2 parts sulfur, 1-2 parts accelerator TMTD, 0.5-1.5 parts accelerator M, 0.5-1.5 parts accelerator TDD, 0.5-1.5 parts accelerator DPTT, 20-40 parts silica, 50-70 parts calcium carbonate, 30-50 parts kaolin, and 1-3 parts paraffin oil.

[0012] Furthermore, the preparation method of the modified natural rubber is as follows: weigh each raw material, mix them, cut the obtained natural rubber compound into particles ≤5cm, and then dissolve them in No. 120 solvent oil. The mass ratio of particles to No. 120 solvent oil is 1:2.5 to obtain the modified natural rubber compound slurry.

[0013] Furthermore, the preparation method of the modified EPDM rubber is as follows: weigh each raw material, mix them, cut the obtained EPDM rubber compound into particles ≤5cm, and then dissolve them in toluene. The mass ratio of particles to toluene is 1:2.5 to obtain the modified EPDM rubber compound slurry.

[0014] Furthermore, the protective suit features a one-piece hood with three hood panels that fit snugly against the face, making it easier to wear breathing equipment.

[0015] Furthermore, the protective suit employs a liquid-tight zipper and a double-layer placket design, effectively enhancing frontal protection.

[0016] Furthermore, the cuffs of the protective suit feature a Velcro elastic band design, allowing for adjustment of the tightness at the wrist according to the thickness of the gloves.

[0017] This invention also provides a method for preparing the above-mentioned hydrofluoric acid protective clothing, comprising the following steps:

[0018] (1) The reverse side of the skeleton fabric is coated with modified natural rubber compound slurry 4 times, each time with a thickness of 0.015 mm, and dried at 80°C; then coated with modified EPDM rubber compound slurry 2 times, each time with a thickness of 0.02 mm, and dried at 80°C.

[0019] (2) The front side of the skeleton fabric is coated with modified natural rubber compound slurry 4 times, each time with a thickness of 0.015mm, and dried at 80℃; then coated with modified EPDM rubber compound slurry 2 times, each time with a thickness of 0.02mm, and dried at 80℃.

[0020] (3) After drying, vulcanization reaction is carried out to obtain protective clothing material.

[0021] Furthermore, the vulcanization reaction is carried out at a temperature of 125-135°C, a pressure of 0.3 MPa, and a time of 180 min.

[0022] As can be seen from the above technical solution, compared with the prior art, the present invention discloses a method for preparing a high-barrier film, with the following beneficial effects:

[0023] (1) The protective clothing of the present invention adopts a multi-component modified rubber material and a multi-layer structure design, with modified natural rubber and modified EPDM rubber as the main protective materials and organic solvent as the carrier. It not only has long-term protection against hydrofluoric acid, but also has the characteristics of high mechanical strength, heat aging resistance, flame retardancy and low temperature softness.

[0024] (2) This invention incorporates a chemical tackifying system into rubber. At the vulcanization temperature, the internal matrix of the rubber reacts to generate a resin adhesive, which then crosslinks on the surface of the reinforcing fabric fibers and the rubber surface, resulting in a chemical reaction. Only the raw materials need to be added during rubber mixing; no additional steps are required. The operation is simple and convenient, and the process is mature. Detailed Implementation

[0025] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0026] Example 1

[0027] A hydrofluoric acid protective suit, the protective suit being made of a 5-layer structure, with a middle layer being a skeleton fabric, and modified natural rubber layer and modified EPDM rubber layer being sequentially arranged on both sides of the skeleton fabric.

[0028] The skeleton fabric is a polyester fabric.

[0029] The modified natural rubber raw materials, by weight, include: 100 parts natural rubber, 3 parts sulfur, 1 part accelerator M, 1 part accelerator DM, 5 parts zinc oxide, 1 part stearic acid, 10 parts silica, 30 parts calcium oxide, 10 parts chlorinated paraffin, 10 parts antimony trioxide, and 1 part antioxidant 4010NA.

[0030] The raw materials for the modified EPDM rubber, by weight, include: 100 parts EPDM rubber, 1.5 parts sulfur, 1.5 parts accelerator TMTD, 1 part accelerator M, 1 part accelerator TDD, 1 part accelerator DPTT, 30 parts silica, 60 parts calcium carbonate, 40 parts kaolin, and 2 parts paraffin oil.

[0031] The method for preparing the modified natural rubber is as follows: weigh each raw material, mix them, cut the resulting natural rubber compound into particles ≤5cm, and then dissolve them in No. 120 solvent oil. The mass ratio of particles to No. 120 solvent oil is 1:2.5 to obtain the modified natural rubber compound slurry.

[0032] The method for preparing the modified EPDM rubber is as follows: weigh each raw material, mix them, cut the resulting EPDM rubber compound into particles ≤5cm, and then dissolve them in toluene. The mass ratio of particles to toluene is 1:2.5 to obtain the modified EPDM rubber compound slurry.

[0033] The protective suit features a one-piece hood with three hood panels that fit snugly against the face, making it easier to wear breathing equipment.

[0034] The protective suit features a liquid-tight zipper and a double-layered placket design, effectively enhancing frontal protection.

[0035] The cuffs of the protective suit feature Velcro elastic bands, allowing for adjustment of the tightness at the wrists based on the thickness of the gloves.

[0036] The above-mentioned method for preparing a hydrofluoric acid protective suit includes the following steps:

[0037] (1) The reverse side of the skeleton fabric is coated with modified natural rubber compound slurry 4 times, each time with a thickness of 0.015 mm, and dried at 80°C; then coated with modified EPDM rubber compound slurry 2 times, each time with a thickness of 0.02 mm, and dried at 80°C.

[0038] (2) The front side of the skeleton fabric is coated with modified natural rubber compound slurry 4 times, each time with a thickness of 0.015mm, and dried at 80℃; then coated with modified EPDM rubber compound slurry 2 times, each time with a thickness of 0.02mm, and dried at 80℃.

[0039] (3) After drying, vulcanization reaction is carried out to obtain protective clothing material.

[0040] The vulcanization reaction was carried out at a temperature of 130°C, a pressure of 0.3 MPa, and a time of 180 min.

[0041] Example 2

[0042] A hydrofluoric acid protective suit, the protective suit being made of a 5-layer structure, with a middle layer being a skeleton fabric, and modified natural rubber layer and modified EPDM rubber layer being sequentially arranged on both sides of the skeleton fabric.

[0043] The skeleton fabric is a polyester fabric.

[0044] The modified natural rubber raw materials, by weight, include: 100 parts natural rubber, 4 parts sulfur, 2 parts accelerator M, 2 parts accelerator DM, 6 parts zinc oxide, 2 parts stearic acid, 15 parts silica, 40 parts calcium oxide, 15 parts chlorinated paraffin, 15 parts antimony trioxide, and 2 parts antioxidant 4010NA.

[0045] The raw materials for the modified EPDM rubber, by weight, include: 100 parts EPDM rubber, 2 parts sulfur, 2 parts accelerator TMTD, 1.5 parts accelerator M, 1.5 parts accelerator TDD, 1.5 parts accelerator DPTT, 40 parts silica, 70 parts calcium carbonate, 50 parts kaolin, and 3 parts paraffin oil.

[0046] The method for preparing the modified natural rubber is as follows: weigh each raw material, mix them, cut the resulting natural rubber compound into particles ≤5cm, and then dissolve them in No. 120 solvent oil. The mass ratio of particles to No. 120 solvent oil is 1:2.5 to obtain the modified natural rubber compound slurry.

[0047] The method for preparing the modified EPDM rubber is as follows: weigh each raw material, mix them, cut the resulting EPDM rubber compound into particles ≤5cm, and then dissolve them in toluene. The mass ratio of particles to toluene is 1:2.5 to obtain the modified EPDM rubber compound slurry.

[0048] The protective suit features a one-piece hood with three hood panels that fit snugly against the face, making it easier to wear breathing equipment.

[0049] The protective suit features a liquid-tight zipper and a double-layered placket design, effectively enhancing frontal protection.

[0050] The cuffs of the protective suit feature Velcro elastic bands, allowing for adjustment of the tightness at the wrists based on the thickness of the gloves.

[0051] The above-mentioned method for preparing a hydrofluoric acid protective suit includes the following steps:

[0052] (1) The reverse side of the skeleton fabric is coated with modified natural rubber compound slurry 4 times, each time with a thickness of 0.015 mm, and dried at 80°C; then coated with modified EPDM rubber compound slurry 2 times, each time with a thickness of 0.02 mm, and dried at 80°C.

[0053] (2) The front side of the skeleton fabric is coated with modified natural rubber compound slurry 4 times, each time with a thickness of 0.015mm, and dried at 80℃; then coated with modified EPDM rubber compound slurry 2 times, each time with a thickness of 0.02mm, and dried at 80℃.

[0054] (3) After drying, vulcanization reaction is carried out to obtain protective clothing material.

[0055] The vulcanization reaction was carried out at a temperature of 135°C, a pressure of 0.3 MPa, and a time of 180 min.

[0056] Example 3

[0057] A hydrofluoric acid protective suit, the protective suit being made of a 5-layer structure, with a middle layer being a skeleton fabric, and modified natural rubber layer and modified EPDM rubber layer being sequentially arranged on both sides of the skeleton fabric.

[0058] The skeleton fabric is a polyester fabric.

[0059] The modified natural rubber raw materials, by weight, include: 100 parts natural rubber, 3 parts sulfur, 1 part accelerator M, 1 part accelerator DM, 4 parts zinc oxide, 1 part stearic acid, 10 parts silica, 20 parts calcium oxide, 5 parts chlorinated paraffin, 5 parts antimony trioxide, and 1 part antioxidant 4010NA.

[0060] The raw materials for the modified EPDM rubber, by weight, include: 100 parts EPDM rubber, 1 part sulfur, 1 part accelerator TMTD, 0.5 parts accelerator M, 0.5 parts accelerator TDD, 0.5 parts accelerator DPTT, 20 parts silica, 50 parts calcium carbonate, 30 parts kaolin, and 1 part paraffin oil.

[0061] The method for preparing the modified natural rubber is as follows: weigh each raw material, mix them, cut the resulting natural rubber compound into particles ≤5cm, and then dissolve them in No. 120 solvent oil. The mass ratio of particles to No. 120 solvent oil is 1:2.5 to obtain the modified natural rubber compound slurry.

[0062] The method for preparing the modified EPDM rubber is as follows: weigh each raw material, mix them, cut the resulting EPDM rubber compound into particles ≤5cm, and then dissolve them in toluene. The mass ratio of particles to toluene is 1:2.5 to obtain the modified EPDM rubber compound slurry.

[0063] The protective suit features a one-piece hood with three hood panels that fit snugly against the face, making it easier to wear breathing equipment.

[0064] The protective suit features a liquid-tight zipper and a double-layered placket design, effectively enhancing frontal protection.

[0065] The cuffs of the protective suit feature Velcro elastic bands, allowing for adjustment of the tightness at the wrists based on the thickness of the gloves.

[0066] The above-mentioned method for preparing a hydrofluoric acid protective suit includes the following steps:

[0067] (1) The reverse side of the skeleton fabric is coated with modified natural rubber compound slurry 4 times, each time with a thickness of 0.015 mm, and dried at 80°C; then coated with modified EPDM rubber compound slurry 2 times, each time with a thickness of 0.02 mm, and dried at 80°C.

[0068] (2) The front side of the skeleton fabric is coated with modified natural rubber compound slurry 4 times, each time with a thickness of 0.015mm, and dried at 80℃; then coated with modified EPDM rubber compound slurry 2 times, each time with a thickness of 0.02mm, and dried at 80℃.

[0069] (3) After drying, vulcanization reaction is carried out to obtain protective clothing material.

[0070] The vulcanization reaction was carried out at a temperature of 130°C, a pressure of 0.3 MPa, and a time of 180 min.

[0071] The performance of the hydrofluoric acid protective clothing obtained in each Example 1 was tested, as shown in Table 1. The chemical penetration resistance time of the fabric was tested using the method in GB 24539-2021 "Protective Clothing - Chemical Protective Clothing".

[0072] Table 1 Performance Tests

[0073]

[0074] In summary, the hydrofluoric acid protective clothing prepared by this invention provides extremely long-lasting protection against high concentrations of hydrofluoric acid, exhibits high mechanical strength, and is suitable for labor operations in the fluorination industry.

[0075] The various embodiments in this specification are described in a progressive manner, with each embodiment focusing on the differences from other embodiments. The same or similar parts between the various embodiments can be referred to each other.

[0076] The above description of the disclosed embodiments enables those skilled in the art to make or use the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A hydrofluoric acid protective suit, characterized in that, The protective suit is made of a 5-layer structure, with a middle layer being a skeleton fabric, and modified natural rubber layer and modified EPDM rubber layer arranged sequentially on both sides of the skeleton fabric. The skeleton fabric is polyester fabric; the raw materials of the modified natural rubber, by weight, include: 100 parts natural rubber, 3-4 parts sulfur, 1-2 parts accelerator M, 1-2 parts accelerator DM, 4-6 parts zinc oxide, 1-2 parts stearic acid, 10-15 parts silica, 20-40 parts calcium oxide, 5-15 parts chlorinated paraffin, 5-15 parts antimony trioxide, and 1-2 parts antioxidant 4010NA; the raw materials of the modified EPDM rubber, by weight, include: 100 parts EPDM rubber, 1-2 parts sulfur, 1-2 parts accelerator TMTD, 0.5-1.5 parts accelerator M, 0.5-1.5 parts accelerator TDD, 0.5-1.5 parts accelerator DPTT, 20-40 parts silica, 50-70 parts calcium carbonate, 30-50 parts kaolin, and 1-3 parts paraffin oil. The method for preparing the modified natural rubber is as follows: weigh each raw material, mix them, cut the resulting natural rubber compound into particles with a particle size ≤ 5cm, and then dissolve them in No. 120 solvent oil. The mass ratio of particles to No. 120 solvent oil is 1:2.5 to obtain the modified natural rubber compound slurry. The method for preparing the modified EPDM rubber is as follows: weigh each raw material, mix them, cut the resulting EPDM rubber compound into particles with a particle size ≤ 5 cm, and then dissolve them in toluene. The mass ratio of particles to toluene is 1:2.5 to obtain the modified EPDM rubber compound slurry.

2. The hydrofluoric acid protective suit according to claim 1, characterized in that, The protective suit is equipped with a one-piece hood and a three-piece cap that fits snugly against the face.

3. The hydrofluoric acid protective suit according to claim 1, characterized in that, The protective suit features a liquid-tight zipper and a double-layered placket design.

4. The method for preparing a hydrofluoric acid protective suit according to claim 1, characterized in that, Includes the following steps: (1) The reverse side of the skeleton fabric is coated with modified natural rubber compound slurry 4 times, each time with a thickness of 0.015 mm, and dried at 80°C; then coated with modified EPDM rubber compound slurry 2 times, each time with a thickness of 0.02 mm, and dried at 80°C. (2) The front side of the skeleton fabric is coated with modified natural rubber compound slurry 4 times, each time with a thickness of 0.015mm, and dried at 80℃; then coated with modified EPDM rubber compound slurry 2 times, each time with a thickness of 0.02mm, and dried at 80℃. (3) After drying, vulcanization reaction is carried out to obtain protective clothing material.

5. The method for preparing a hydrofluoric acid protective suit according to claim 4, characterized in that, The vulcanization reaction was carried out at a temperature of 125-135℃, a pressure of 0.3MPa, and a time of 180min.

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