A high-performance sealing material and its application in leak prevention

By introducing modified attapulgite and organophosphorus flame retardants into polyester elastomers, the problems of easy corrosion and flammability of polyester elastomers have been solved, achieving acid and alkali resistance and flame retardancy of high-performance sealing materials, thus improving the safety and environmental performance of chemical enterprises.

CN116790098BActive Publication Date: 2025-11-14ANHUI JIESURI IND EQUIP CO LTD
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Patent Information

Application Number
CN202310752425.7
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-06-26
Publication Date
2025-11-14
Estimated Expiration
2043-06-26

AI Technical Summary

Technical Problem

Polyester elastomers are easily corroded by acids and alkalis in chemical production, which leads to a decline in sealing performance. They are also flammable and pose a risk of fire and explosion.

Method used

A high-performance sealing material is prepared by using modified attapulgite as an inorganic filler and grafting phosphorus-containing flame retardants onto its surface. This forms a stable physical barrier layer, improves acid and alkali resistance, and achieves flame retardant effect by generating phosphoric acid derivatives through organophosphorus flame retardants.

Benefits of technology

It improves the acid and alkali resistance and flame retardant properties of sealing materials, reduces the risk of safety accidents and environmental pollution in chemical enterprises, and ensures sealing effect and production safety.

✦ Generated by Eureka AI based on patent content.

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Abstract

This invention relates to the field of composite material technology and discloses a high-performance sealing material and its application in preventing leakage. The sealing material includes a base plate material and a dust-adhesive plate material. The base plate material includes a polyester elastomer and a modified inorganic filler. The dust-adhesive plate material includes a TPU polyether elastomer, a flame retardant, and a vulcanizing agent. By grafting an organophosphorus flame retardant onto the surface of attapulgite clay and then using it as an inorganic filler in the preparation of the base plate material, the sealing material possesses excellent acid and alkali resistance and flame retardant properties, preventing chemical leakage and effectively reducing the possibility of safety accidents and environmental pollution in chemical enterprises, thereby further improving the safety production level of chemical enterprises.
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Description

Technical Field

[0001] This invention relates to the field of composite material technology, and more specifically to a high-performance sealing material and its application in preventing leakage. Background Technology

[0002] With the rapid development of chemical enterprises, environmental pollution has become a common concern. Chemical waste liquids generated during chemical production contain a large number of toxic and harmful substances, such as heavy metal ions, organic matter, and cyanides. If these pollutants are discharged into the ground through sewers and sewage outlets, they will cause serious pollution to groundwater and threaten people's health. Therefore, it is particularly important to properly store chemicals and treat chemical waste liquids. Using high-performance sealing materials to prevent chemical leakage is essential for chemical enterprises.

[0003] Currently, commonly used sealing materials include nitrile rubber, hydrogenated nitrile rubber, fluororubber, polyurethane, polytetrafluoroethylene, and polyacrylate. Patent application CN201310592715.6 discloses a rubber sealing material with high mechanical strength, low coefficient of friction, strong wear resistance, and long service life under high temperature and pressure. Patent application CN201611130349.2 discloses a high-performance nitrile rubber sealing material and its preparation method. This high-performance nitrile rubber sealing material solves the problems of poor wear resistance, low tensile strength, and low tear strength of ordinary nitrile rubber, and the prepared product has strong mechanical properties and excellent high-temperature resistance.

[0004] Polyester elastomers are widely used in the chemical industry as a leak-proof sealing material due to their excellent water resistance, oil resistance, high toughness, and abrasion resistance. However, chemical production processes use many acidic and alkaline reagents, which can easily corrode polyester elastomers, leading to a decrease in their sealing performance, causing chemicals to leak everywhere, and potentially causing fires.

[0005] Furthermore, polyester elastomers are highly flammable, and in the event of a fire, there is a risk of chemical explosion. Therefore, this invention has developed a high-performance sealing material and produced two typical products: overflow dikes and drainage well protective mats, which are used in the field of seepage prevention. Summary of the Invention

[0006] The purpose of this invention is to provide a high-performance sealing material that solves the problems of poor acid and alkali resistance and flame retardancy of polyester elastomers as sealing materials.

[0007] The objective of this invention can be achieved through the following technical solutions:

[0008] A high-performance sealing material, comprising a base plate material and a dust-adhesive plate material; the base plate material comprises the following raw materials in parts by weight: 40-50 parts polyester elastomer, 5-8 parts modified inorganic filler; the modified inorganic filler is attapulgite clay with a phosphorus-containing flame retardant grafted onto its surface; the dust-adhesive plate material comprises the following raw materials in parts by weight: 30-40 parts TPU polyether elastomer, 10-12 parts flame retardant, 4-6 parts vulcanizing agent.

[0009] Furthermore, the flame retardant is either trimethylolphosphine oxide or dimethyl methyl phosphate.

[0010] Furthermore, the vulcanizing agent is either sulfur or benzoyl peroxide.

[0011] Furthermore, the preparation method of the modified inorganic filler includes the following steps:

[0012] A: Mix attapulgite with tetrahydrofuran, ultrasonically disperse for 0.5-1h, add succinyl chloride and acid-binding agent, stir evenly, purge with nitrogen, and react at room temperature for 12-14h. After the reaction is complete, centrifuge to separate the solid material to obtain attapulgite intermediate.

[0013] B: Disperse the attapulgite intermediate in toluene, sonicate for 0.5-1 h, raise the temperature to 80-90℃, add diethyl phosphite, stir and react for 10-12 h. After the reaction is complete, centrifuge to separate the solid product, wash and vacuum dry to obtain modified attapulgite.

[0014] Furthermore, in step A, the mesh size of the attapulgite soil is 200-300 mesh.

[0015] Further, in step A, the acid-binding agent is triethylamine.

[0016] Through the above technical solution, the succinyl chloride structure contains a highly reactive acyl chloride group, which can react with the hydroxyl groups on the surface of attapulgite. The acyl chloride group is modified onto the surface of attapulgite, and then the phosphorus-hydrogen bond in diethyl phosphite is easily broken, reacting with the acyl chloride group on the surface of attapulgite to graft the organophosphorus flame retardant diethyl phosphite into the structure of attapulgite, thus obtaining a modified inorganic filler.

[0017] Furthermore, the specific method for preparing the base plate material is as follows:

[0018] Mix the polyester elastomer and modified inorganic filler in parts by weight evenly, raise the temperature to 60-70℃, stir for 4-5 hours at a speed of 1200-1400 r / min, then pour into a mold at 40-50℃, cure for 12-24 hours, remove the mold, and obtain the base plate material.

[0019] Furthermore, the method for preparing the sealing material includes the following steps:

[0020] Step 1: Mix the TPU polyether elastomer and flame retardant evenly in parts by weight, raise the temperature to 70-80℃, stir for 3-5 hours at a speed of 1200-1400r / min, then add the vulcanizing agent and stir evenly to obtain the dust-adhesive board material.

[0021] Step 2: Pour the adhesive board material onto one side of the base plate material, then inject it into the mold. Vulcanize for 50-60 minutes at a temperature of 140-150℃ and a pressure of 8-10MPa. After cooling to room temperature, remove the mold. Then, vulcanize a second time at a temperature of 110-120℃ and a pressure of 8-10MPa for 10-12 hours. After cooling to room temperature, demold to obtain the sealing material.

[0022] The beneficial effects of this invention are:

[0023] This invention develops a high-performance sealing material to produce two typical products for seepage prevention: overflow dikes and drainage well protective mats. The overflow dikes are mainly placed around chemical drums or machines to control the leakage range and prevent the waste liquid from spreading. The drainage well protective mats are mainly placed at sewage outlets or sewer openings to prevent waste liquid and other pollutants from flowing into important areas such as groundwater. Both have high sealing performance and can adhere tightly to the ground even in places with fine sand, stones, or uneven surfaces.

[0024] This invention incorporates organically modified attapulgite as an inorganic filler during the preparation of the base plate material. After organic modification, the surface properties of the attapulgite change from hydrophilic to oleophilic, thus exhibiting good interfacial compatibility with polyester elastomers. This facilitates the uniform dispersion of the inorganic filler within the base plate material. Utilizing the unique lamellar structure of attapulgite, a stable physical barrier layer is formed within the base plate material, extending the diffusion path of corrosive media such as acids and alkalis. This improves the acid and alkali resistance of the base plate material, resulting in superior sealing performance, preventing chemical leakage, and effectively reducing the risk of chemical spills in chemical plants. On the one hand, there is the possibility of safety accidents and environmental pollution. On the other hand, the organophosphorus flame retardant introduced on the surface of attapulgite can generate phosphoric acid derivatives during combustion. These phosphoric acid derivatives have a strong dehydration ability, which can not only carbonize the surface of the sealing material and delay the entry of oxygen and heat into the interior of the sealing material, but also the released water vapor has an endothermic effect, reducing the oxidation heat of the sealing material surface and achieving the purpose of condensed phase flame retardancy. At the same time, attapulgite itself has flame retardant properties, and its layered structure can effectively isolate oxygen and heat, thereby improving the flame retardant performance of the sealing material and further improving the safety production level of chemical enterprises.

[0025] Of course, any product implementing this invention does not necessarily need to achieve all of the advantages described above at the same time. Attached Figure Description

[0026] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0027] Figure 1 Thermogravimetric curves of attapulgite, attapulgite intermediate, and modified attapulgite.

[0028] Figure 2 This is a diagram illustrating the overflow prevention dike.

[0029] Figure 3 This is a diagram showing the protective pad for the drainage well. Detailed Implementation

[0030] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. 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.

[0031] Example 1

[0032] I. Preparation of Modified Inorganic Fillers

[0033] A: Mix 2g of attapulgite with 80mL of tetrahydrofuran, ultrasonically disperse for 0.5h, add 1.6g of succinyl chloride and 1.2g of triethylamine, stir evenly, purge with nitrogen, and react at room temperature for 12h. After the reaction is complete, centrifuge to separate the solid material to obtain the attapulgite intermediate.

[0034] B: Disperse 1g of attapulgite intermediate in 100mL of toluene, sonicate for 0.5h, raise the temperature to 80℃, add 1.4g of diethyl phosphite, stir and react for 10h. After the reaction is complete, centrifuge to separate the solid product, wash and vacuum dry to obtain modified attapulgite.

[0035] Weigh 0.5g of attapulgite, attapulgite intermediate, and modified attapulgite samples respectively, and place them in an SDTQ600 thermogravimetric analyzer. Under a nitrogen atmosphere, the temperature was increased from 25℃ to 600℃ at a heating rate of 10℃ / min for thermogravimetric analysis. The results are as follows. Figure 1 As shown, by Figure 1It can be seen that the final residual weight of attapulgite is 85.3% because the adsorbed water, crystal water on its surface, and zeolite water in the internal pores of its structure decompose under high temperature conditions. After the intermediate of attapulgite is decomposed at high temperature, the final residual weight is 55.6% due to the decomposition of the acyl chloride grafted on its surface. The final residual weight of modified attapulgite is 23.2% due to the pyrolysis of the alkyl chains and phosphorous organic matter introduced into the structure of modified attapulgite.

[0036] II. Preparation of base plate material

[0037] Mix 40 parts of polyester elastomer and 5 parts of modified inorganic filler evenly, raise the temperature to 60°C, stir for 4 hours at a speed of 1200 r / min, then pour into a mold at 40°C, cure for 12 hours, remove the mold, and obtain the base plate material.

[0038] Example 2

[0039] Preparation of base plate material

[0040] 45 parts of polyester elastomer and 6 parts of modified inorganic filler were mixed evenly, the temperature was raised to 65℃, and the mixture was stirred for 4.5 hours at a speed of 1300 r / min. Then the mixture was poured into a mold at 45℃ and cured for 18 hours. The mold was then removed to obtain the base plate material.

[0041] The preparation method of the modified inorganic filler is the same as that in Example 1.

[0042] Example 3

[0043] Preparation of base plate material

[0044] Mix 50 parts of polyester elastomer and 8 parts of modified inorganic filler evenly, raise the temperature to 70°C, stir for 5 hours at a speed of 1400 r / min, then pour into a mold at 50°C, cure for 24 hours, remove the mold, and obtain the base plate material.

[0045] The preparation method of the modified inorganic filler is the same as that in Example 1.

[0046] Comparative Example 1

[0047] Preparation of base plate material

[0048] Mix 50 parts of polyester elastomer and 8 parts of attapulgite evenly, raise the temperature to 70°C, stir for 5 hours at a speed of 1400 r / min, then pour into a mold at 50°C, cure for 24 hours, remove the mold, and obtain the base plate material.

[0049] Comparative Example 2

[0050] Preparation of base plate material

[0051] 50 parts of polyester elastomer were poured into a mixer, the temperature was raised to 70°C, and the mixture was stirred for 5 hours at a speed of 1400 r / min. Then it was poured into a mold at 50°C and cured for 24 hours. The mold was then removed to obtain the base plate material.

[0052] Performance testing

[0053] ① The base plate materials prepared in Examples 1-3 and Comparative Examples 1-2 of this invention were cut into 50mm×10mm samples. The samples were then immersed in a 20% (v / v) sulfuric acid solution and a 30% (w / w) sodium hydroxide solution at room temperature. The time required for the samples to exhibit changes in properties such as blistering and deformation was recorded to evaluate the acid and alkali resistance of the base plate materials. The test results are shown in the table below:

[0054]

[0055] As can be seen from the table above, the base plate materials prepared in Examples 1-3 of the present invention require a long time to undergo property changes in acid and alkali solutions, thus exhibiting excellent acid and alkali resistance. The sealing material prepared in Comparative Example 1 has better acid and alkali resistance due to the addition of attapulgite, while the base plate material prepared in Comparative Example 2 has poorer acid and alkali resistance because it does not contain attapulgite.

[0056] ② Referring to the national standard GB / T 2406.2-2009 "Determination of Combustion Behavior of Plastics by Oxygen Index Method", the combustion performance of the base plate materials prepared in Examples 1-3 and Comparative Examples 1-2 of this invention was tested. The test results are shown in the table below:

[0057]

[0058] As can be seen from the table above, the base plate materials prepared in Examples 1-3 of the present invention have excellent flame retardant properties. The base plate material prepared in Comparative Example 1 did not introduce organophosphorus flame retardants, but added attapulgite, so its flame retardant properties were average. The sealing material prepared in Comparative Example 2 did not introduce organophosphorus flame retardants, nor did it add attapulgite, so its flame retardant properties were poor.

[0059] Sealing materials were prepared using the base plate materials prepared in Examples 1-3, and the preparation methods included the following steps:

[0060] Step 1: Mix 30 parts of TPU polyether elastomer and 10 parts of dimethyl methyl phosphate evenly, raise the temperature to 70°C, stir for 3 hours at a speed of 1200 r / min, then add 4 parts of sulfur and stir evenly to obtain the dust-adhesive board material.

[0061] Step 2: Pour the adhesive board material onto one side of the base plate material, then inject it into the mold. Vulcanize for 60 minutes at a temperature of 140℃ and a pressure of 8MPa. After cooling to room temperature, remove the mold. Then, vulcanize a second time at a temperature of 110℃ and a pressure of 8MPa for 10 hours. After cooling to room temperature, demold to obtain the sealing material.

[0062] Application of high-performance sealing materials in leak prevention

[0063] Application 1

[0064] like Figure 2 As shown, a high-performance sealing material used in the field of seepage prevention is a spill containment dike. The spill containment dike is mainly used around chemical drums or machinery to control the leakage range and prevent waste liquid from further flowing into important areas such as groundwater. It has a high sealing degree and can adhere tightly to the ground even in places with fine sand, stones, or uneven surfaces. The dike is also expandable and can fit snugly against any corner or curved surface. Its interlocking design allows for easy connection to contain large-area leaks. It is reusable and can be cleaned with soap and water. The prominent yellow design serves as a warning of liquid spills, reducing the possibility of tripping.

[0065] Application 2

[0066] like Figure 3 As shown, a high-performance sealing material used in the field of seepage prevention is a drainage well protective pad. This pad is mainly placed at sewage outlets or sewer openings to prevent waste liquids and other pollutants from flowing into important areas such as groundwater. It has a high sealing degree, adhering tightly to the ground even in areas with fine sand, pebbles, or uneven surfaces. The pad is expandable and can fit snugly against any corner or curved surface, blocking leaks without absorbing them. It is reusable and can be cleaned with soap and water. Its bright yellow design alerts users to potential spills, reducing the possibility of tripping. When covering a drainage well, the protective pad should overlap the well opening by at least 8cm on each side. It is durable, with a typical product lifespan of 5 years, and can withstand the weight of forklifts and heavy trucks.

[0067] The models and specifications of the manufactured overflow dikes and drainage well protective mats are shown in the table below:

[0068]

[0069] At room temperature, 20% sulfuric acid solution (v / v), 30% sodium hydroxide solution (w / w), ethylene glycol, glycerin, dimethyl silicone oil, and N,N-dimethylformamide were poured into a ring-shaped dike formed by an overflow prevention dike. Leakage was observed after 1 day, 3 days, and 7 days. A drainage well protective mat was attached to a filter screen, and at room temperature, 20% sulfuric acid solution (v / v), 30% sodium hydroxide solution (w / w), ethylene glycol, glycerin, dimethyl silicone oil, and N,N-dimethylformamide were poured into the protective mat. Leakage was observed after 1 day, 3 days, and 7 days. After 1 day and 7 days, tests were conducted to check for leakage. A 20% sulfuric acid solution (by volume), a 30% sodium hydroxide solution (by mass), ethylene glycol, glycerin, dimethyl silicone oil, and N,N-dimethylformamide were poured into the overflow dike for 1 day, 3 days, and 7 days respectively. No leakage was observed in the overflow dike. Similarly, after pouring the same 20% sulfuric acid solution (by volume), 30% sodium hydroxide solution (by mass), ethylene glycol, glycerin, dimethyl silicone oil, and N,N-dimethylformamide) into the protective mat for 1 day, 3 days, and 7 days respectively, no leakage was observed in the filter screen below the protective mat in the drainage well.

[0070] The above content is merely an example and illustration of the concept of the present invention. Those skilled in the art can make various modifications or additions to the specific embodiments described, or use similar methods to replace them, as long as they do not deviate from the concept of the invention or exceed the scope defined in the claims, and all such modifications and additions should fall within the protection scope of the present invention.

Claims

1. A high-performance sealing material, characterized in that, The sealing material includes a base plate material and a dust-adhesive plate material; the base plate material includes the following raw materials in parts by weight: 40-50 parts polyester elastomer and 5-8 parts modified inorganic filler; The modified inorganic filler is attapulgite clay with a phosphorus-containing flame retardant grafted onto its surface; the dust-adhesive board material comprises the following raw materials in parts by weight: 30-40 parts TPU polyether elastomer, 10-12 parts flame retardant, and 4-6 parts vulcanizing agent. The preparation method of the modified inorganic filler includes the following steps: A: Mix attapulgite with tetrahydrofuran, ultrasonically disperse for 0.5-1h, add succinyl chloride and acid-binding agent, stir evenly, purge with nitrogen, and react at room temperature for 12-14h. After the reaction is complete, centrifuge to separate the solid material to obtain attapulgite intermediate. B: Disperse the attapulgite intermediate in toluene, sonicate for 0.5-1 h, raise the temperature to 80-90℃, add diethyl phosphite, stir and react for 10-12 h. After the reaction is complete, centrifuge to separate the solid product, wash and vacuum dry to obtain modified attapulgite.

2. The high-performance sealing material according to claim 1, characterized in that, In step A, the mesh size of the attapulgite soil is 200-300 mesh.

3. The high-performance sealing material according to claim 1, characterized in that, In step A, the acid-binding agent is triethylamine.

4. The high-performance sealing material according to claim 1, characterized in that, The flame retardant is either trimethylolphosphine oxide or dimethyl methyl phosphate.

5. The high-performance sealing material according to claim 1, characterized in that, The vulcanizing agent is either sulfur or benzoyl peroxide.

6. The high-performance sealing material according to claim 1, characterized in that, The specific method for preparing the base plate material is as follows: Mix the polyester elastomer and modified inorganic filler in parts by weight evenly, raise the temperature to 60-70℃, stir for 4-5 hours at a speed of 1200-1400 r / min, then pour into a mold at 40-50℃, cure for 12-24 hours, remove the mold, and obtain the base plate material.

7. The high-performance sealing material according to claim 1, characterized in that, The method for preparing the sealing material includes the following steps: Step 1: Mix the TPU polyether elastomer and flame retardant evenly in parts by weight, raise the temperature to 70-80℃, stir for 3-5 hours at a speed of 1200-1400r / min, then add the vulcanizing agent and stir evenly to obtain the dust-adhesive board material. Step 2: Pour the adhesive board material onto one side of the base plate material, then inject it into the mold. Vulcanize for 50-60 minutes at a temperature of 140-150℃ and a pressure of 8-10MPa. After cooling to room temperature, remove the mold. Then, vulcanize a second time at a temperature of 110-120℃ and a pressure of 8-10MPa for 10-12 hours. After cooling to room temperature, demold to obtain the sealing material.

Citation Information

Patent Citations

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    CN103588938B

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