WO2019227535A1 - High-temperature resistant, soft and flexible sealing gasket, preparation method thereof, and use thereof - Google Patents

High-temperature resistant, soft and flexible sealing gasket, preparation method thereof, and use thereof Download PDF

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WO2019227535A1
WO2019227535A1 PCT/CN2018/091743 CN2018091743W WO2019227535A1 WO 2019227535 A1 WO2019227535 A1 WO 2019227535A1 CN 2018091743 W CN2018091743 W CN 2018091743W WO 2019227535 A1 WO2019227535 A1 WO 2019227535A1
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Prior art keywords
fiber cloth
binder slurry
refractory fiber
gasket
parts
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PCT/CN2018/091743
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French (fr)
Chinese (zh)
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刘开琪
孙广超
熊瑞
陈运法
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中国科学院过程工程研究所
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B33/00Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/22Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
    • B32B5/24Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
    • B32B5/26Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04Interconnection of layers
    • B32B7/12Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04Polyurethanes
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M17/00Producing multi-layer textile fabrics
    • D06M17/04Producing multi-layer textile fabrics by applying synthetic resins as adhesives
    • D06M17/10Polyurethanes polyurea
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00Properties of the layers or laminate
    • B32B2307/30Properties of the layers or laminate having particular thermal properties
    • B32B2307/306Resistant to heat
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00Properties of the layers or laminate
    • B32B2307/70Other properties
    • B32B2307/714Inert, i.e. inert to chemical degradation, corrosion
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium

Definitions

  • the filler comprises any one or a combination of at least two of vermiculite particles, mullite short fibers, or zirconia short fibers.
  • Typical but non-limiting combinations are: a combination of vermiculite particles and mullite short fibers, a combination of mullite short fibers and zirconia short fibers, a combination of vermiculite particles and zirconia short fibers, vermiculite particles, A combination of short stone fibers and short zirconia fibers.
  • the length of the short fibers is 100-500 ⁇ m.
  • step (2) the method of processing and forming is die cutting.
  • the high-temperature-resistant flexible elastic gaskets provided in the present disclosure have readily available raw materials, are environmentally friendly, have simple preparation processes, and are suitable for industrial applications.
  • FIG. 1 is a schematic cross-sectional view (not limited to the number of superimposed layers) of the gasket prepared in Example 1 of the present disclosure, where 1-refractory fiber cloth, 2-binder slurry;
  • the binder slurry component and the mixing ratio of the sealing material are selected as: 68 parts of water-based polyurethane, 16 parts of epoxy resin emulsion, 15 parts of filler, 1 part of aluminum sol, and 1 part of dispersant. .
  • the test results show that the gasket prepared in this embodiment has the flexibility of tightly combining with the sealing surface, plays a role of flexible elastic sealing and buffering stress, and can be used for a long time in an environment of 700-1000 ° C. After a long-term temperature resistance test, it was found that it has a good sealing effect, high integrity and high strength at high temperatures, does not adhere to the surface of the pipe, can be quickly cleaned, and is easy to disassemble and replace. Ceramic membrane filter tubes that can be used for high temperature flue gas purification, such as steel plant flue gas purification and other industrial high temperature flue gas purification equipment.
  • the three-layer stacked gasket prepared in this embodiment is used at 700 ° C. for a long time, and the tensile strength is maintained at about 27.5 MPa.
  • the test results show that the gasket prepared in this embodiment has the flexibility of tightly combining with the sealing surface, plays a role of flexible elastic sealing and buffering stress, and can be used for a long time in an environment of 700-1000 ° C. After a long-term temperature resistance test, it was found that it has a good sealing effect, high integrity and high strength at high temperatures, does not adhere to the surface of the pipe, can be quickly cleaned, and is easy to disassemble and replace. Ceramic membrane filter tubes that can be used for high temperature flue gas purification, such as steel plant flue gas purification and other industrial high temperature flue gas purification equipment.

Abstract

The present invention provides a high-temperature resistant, soft and flexible sealing gasket, a preparation method thereof, and a use thereof. The sealing gasket includes heat-resistant fiber fabric members and a binder slurry. The heat-resistant fiber fabric members are laminated on each other. The binder slurry is provided between adjacent heat-resistant fiber fabric members and at an outer side of the outermost heat-resistant fiber fabric member. The binder slurry comprises the following components, in parts by weight: 50-70 parts of aqueous polyurethane, 10-35 parts of epoxy resin emulsion, 10-15 parts of filler, 1-5 parts of aluminium sol-gel, and 0.5-1 parts of dispersant. The preparation method comprises: 1) preparing a binder slurry; 2) adding the binder slurry from step 1) to adhesion surfaces of heat-resistant fiber fabric members, laminating the heat-resistant fiber fabric members that have been combined with the binder slurry, and molding the same to obtain a sealing gasket. The high-temperature resistant, soft and flexible sealing gasket of the present invention can be used in a high temperature environment for a long time.

Description

一种耐高温的柔弹性密封垫及其制备方法和用途High-temperature-resistant flexible elastic gasket and preparation method and application thereof 技术领域Technical field
本公开属于无机非金属复合材料领域,具体涉及一种耐高温的柔弹性密封垫及其制备方法和用途。The present disclosure belongs to the field of inorganic non-metal composite materials, and particularly relates to a high-temperature-resistant flexible elastic gasket and a preparation method and application thereof.
背景技术Background technique
近年来,随着石油化工、冶金、环境保护等行业的不断发展,对高温含尘气体分离装置的耐高温高压性能提出了越来越高的要求,而高温密封技术一直是影响装置能否长时间连续运行的重要因素之一。在工业生产过程中,使用环境温度与密封材料不符或者在热过载状态下,都会加速密封材料的老化、脆化等等,高温工况下管件的密封技术显得尤为重要,这也对密封材料的耐温性能和密封性能提出更为苛刻的要求。In recent years, with the continuous development of petrochemical, metallurgy, environmental protection and other industries, higher and higher requirements for the high temperature and high pressure resistance of high-temperature dust-containing gas separation devices have been put forward. One of the important factors of continuous time operation. In the industrial production process, the use of environmental temperature that does not match the sealing material or under thermal overload conditions will accelerate the aging, embrittlement, etc. of the sealing material. The sealing technology of the pipe under high temperature conditions is particularly important, which is also important for the sealing material. Temperature resistance and sealing performance put forward more demanding requirements.
针对600℃以下的柔弹性密封技术较为成熟,但是在700~1000℃高温下长期使用的耐高温柔弹性密封材料的开发还较为匮乏。The flexible and elastic sealing technology below 600 ℃ is relatively mature, but the development of high-temperature resistant flexible and elastic sealing materials that have been used for a long time at a high temperature of 700 ~ 1000 ℃ is still lacking.
CN106188897A公开了一种耐高温乙丙橡胶密封垫片及其制备方法和应用,该方案中,耐高温乙丙橡胶密封垫片由二元乙丙橡胶、炉法炭黑、喷雾炭黑、氧化锌、氧化铝、硫化剂、助交联剂和防老剂等组成,其中采用完全饱和的二元乙丙橡胶作为橡胶原料。CN106188897A discloses a high-temperature-resistant ethylene-propylene rubber gasket and a preparation method and application thereof. In this solution, the high-temperature-resistant ethylene-propylene rubber gasket is composed of a binary ethylene-propylene rubber, furnace black, spray carbon black, and zinc oxide. , Alumina, vulcanizing agent, cross-linking agent and antioxidant, etc., which uses fully saturated ethylene-propylene rubber as the rubber raw material.
CN204852334U公开了一种高温密封石墨垫片,该石墨垫片包括有金属内环和金属外环,所述金属内环与金属外环之间嵌设有石墨环,所述石墨环的厚度高于金属内环和金属外环的厚度,所述金属内环为弧形内凹结构,所述金属外环为弧形外凸结构,所述石墨环设有与金属内环和金属外环贴合的弧形凸起。CN204852334U discloses a high-temperature sealed graphite gasket. The graphite gasket includes a metal inner ring and a metal outer ring. A graphite ring is embedded between the metal inner ring and the metal outer ring. The thickness of the graphite ring is greater than The thickness of the metal inner ring and the metal outer ring. The metal inner ring is an arc-shaped concave structure, the metal outer ring is an arc-shaped convex structure, and the graphite ring is provided with a metal inner ring and a metal outer ring. Curved protrusions.
CN202684067U公开了一种耐火纤维密封垫,该耐火纤维密封垫采用耐火纤 维材质,表面具有优良的弹性,适合不断变化的塞棒水口形状,能有效地进行塞棒水口的堵塞密封。CN202684067U discloses a refractory fiber gasket. The refractory fiber gasket is made of refractory fiber material and has excellent elasticity on the surface. It is suitable for changing the shape of the plug nozzle, and can effectively seal the plug nozzle.
但是上述三个方案均无法在700~1000℃高温下长期使用。However, the above three solutions cannot be used for a long time at a high temperature of 700 to 1000 ° C.
高温含尘烟气净化技术中异质管件间的高温密封,通常使用耐火纤维棉、毡进行填充密封,但由于纤维棉、毡质地松软、强度低、连续性差,使得在安装过程中易于发生破损,造成受力不均,密封效果差。在长时间的高温运行及反吹过程的机械振动下,由于材料的耐温性差,造成老化严重,易发生气体泄漏,对高温含尘烟气净化效率有很大的不利影响。为了解决此技术问题,急需开发一种高强度的耐高温柔弹性密封材料。In the high-temperature dust-containing flue gas purification technology, high-temperature seals between heterogeneous pipe fittings are usually filled and sealed with refractory fiber cotton and felt, but because of the soft texture, low strength, and poor continuity of fiber cotton and felt, it is easy to break during installation , Resulting in uneven force, poor sealing effect. Under long-term high-temperature operation and mechanical vibration during the backflushing process, due to the poor temperature resistance of the material, the aging is severe, and gas leakage is prone to occur, which has a great adverse effect on the purification efficiency of high-temperature dusty flue gas. In order to solve this technical problem, it is urgent to develop a high-strength, high-temperature-resistant, flexible and elastic sealing material.
发明内容Summary of the Invention
以下是对本公开详细描述的主题的概述。本概述并非是为了限制权利要求的保护范围。The following is an overview of the subject matter described in detail in this disclosure. This summary is not intended to limit the scope of protection of the claims.
针对现有技术中存在的密封材料在高温下易粉化、密封效果不佳、机械强度低、寿命较短等问题,本公开的目的在于提供一种耐高温的柔弹性密封垫及其制备方法和用途。本公开提供的耐高温的柔弹性密封垫可以在高温环境中长期使用。Aiming at the problems in the prior art that sealing materials are easily powdered at high temperatures, have poor sealing effects, low mechanical strength, and short life, the purpose of this disclosure is to provide a high-temperature-resistant flexible elastic gasket and a method for preparing the same. And uses. The high-temperature-resistant flexible elastic gasket provided by the present disclosure can be used for a long time in a high-temperature environment.
为达上述目的,本公开采用以下技术方案:To achieve the above purpose, the present disclosure adopts the following technical solutions:
第一方面,本公开提供一种密封垫,所述密封垫包括耐火纤维布和结合剂浆料,所述耐火纤维布相互叠加,所述结合剂浆料位于相邻的耐火纤维布之间以及最外层耐火纤维布的外侧面;In a first aspect, the present disclosure provides a gasket including a refractory fiber cloth and a binder slurry, the refractory fiber cloth is superimposed on each other, and the binder slurry is located between adjacent refractory fiber cloths and The outer side of the outermost refractory fiber cloth;
所述结合剂浆料以重量份计包括以下组分:The binder slurry includes the following components in parts by weight:
Figure PCTCN2018091743-appb-000001
Figure PCTCN2018091743-appb-000001
Figure PCTCN2018091743-appb-000002
Figure PCTCN2018091743-appb-000002
本公开中,所述结合剂浆料以重量份计,水性聚氨酯的重量份数为50~70份,例如50份、52份、55份、57份、60份、62份、65份、68份或70份等,但并不仅限于所列举的数值,该数值范围内其他未列举的数值同样适用。In the present disclosure, the binder slurry is 50 to 70 parts by weight, such as 50 parts, 52 parts, 55 parts, 57 parts, 60 parts, 62 parts, 65 parts, 68 parts by weight. Parts or 70 parts, etc., but it is not limited to the listed values, and other unlisted values within this range are also applicable.
环氧树脂乳液的重量份数为10~35份,例如10份、13份、16份、18份、20份、22份、25份、28份、30份、33份或35份等,但并不仅限于所列举的数值,该数值范围内其他未列举的数值同样适用。The weight of the epoxy resin emulsion is 10 to 35 parts, for example, 10 parts, 13 parts, 16 parts, 18 parts, 20 parts, 22 parts, 25 parts, 28 parts, 30 parts, 33 parts, or 35 parts, etc., but It is not limited to the listed values, and other unlisted values within the range are also applicable.
填料的重量份数为10~15份,例如10份、11份、12份、13份、14份或15份等,但并不仅限于所列举的数值,该数值范围内其他未列举的数值同样适用。The weight parts of the filler are 10-15 parts, for example, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, or 15 parts, etc., but it is not limited to the listed values, and other unlisted values in the range are the same Be applicable.
铝溶胶的重量份数为1~5份,例如1份、2份、3份、4份或5份等,但并不仅限于所列举的数值,该数值范围内其他未列举的数值同样适用。The weight fraction of the aluminum sol is 1 to 5 parts, for example, 1 part, 2 parts, 3 parts, 4 parts, or 5 parts, etc., but it is not limited to the listed values, and other unlisted values in this range are also applicable.
分散剂的重量份数为0.5~1份,例如0.5份、0.6份、0.7份、0.8份、0.9份或1份等,但并不仅限于所列举的数值,该数值范围内其他未列举的数值同样适用。The weight part of the dispersant is 0.5 to 1 part, for example, 0.5 part, 0.6 part, 0.7 part, 0.8 part, 0.9 part, or 1 part, etc., but it is not limited to the listed values, and other unlisted values within this value range The same applies.
本公开提供的密封垫中,通过结合剂浆料和耐火纤维布的协同作用,互相配合,使得密封垫的整体性能得到显著增强。具体来讲,本公开通过将水性聚氨酯、环氧树脂乳液、蛭石颗粒、莫来石短纤维、氧化锆短纤维、铝溶胶、分散剂混合,形成结合剂浆料,在保证粘性和环保性的同时,有效地提高了材料的机械强度,常温下强度高、不硬化,高温下柔性好、不脆断,能更好地满足材料的高温柔弹性;通过耐火纤维布的多层复合,使材料具有高机械强度,同时,多层纤维可在压力和热应力下自调适所受到的刚性点应力,通过缝隙补偿 及优良的抗腐蚀性,提高材料的密封性能。In the gasket provided by the present disclosure, the synergy between the binder slurry and the refractory fiber cloth cooperates with each other, so that the overall performance of the gasket is significantly enhanced. Specifically, the present disclosure forms a binder slurry by mixing water-based polyurethane, epoxy resin emulsion, vermiculite particles, mullite short fibers, zirconia short fibers, aluminum sol, and dispersant to ensure adhesiveness and environmental protection. At the same time, it effectively improves the mechanical strength of the material. It has high strength at normal temperature, does not harden, and has good flexibility and brittleness at high temperature, which can better meet the high temperature flexibility of the material. The material has high mechanical strength. At the same time, the multilayer fiber can self-adjust the rigid point stress it receives under pressure and thermal stress. Through gap compensation and excellent corrosion resistance, the material's sealing performance is improved.
本公开中的耐高温柔弹性密封垫与普通耐火纤维棉、毡相比,具有强度高、厚度均匀、连续性好等优越性能,能够承受脉冲反吹清灰时引起的轴向振动,并且能缓冲陶瓷膜与钢板之间的热应力作用,提供可靠的固定连接和密封性能,且其自身还具有制作工艺简单,成本低廉等优势。更重要的是,复合材料制品的种类具有多种形式,可以制成各种形状、尺寸、厚度等,具有热传导率低、不燃烧、强度重量比高、化学稳定性好、高温下保持较好的柔弹性等特点。本公开提供的耐高温的柔弹性密封垫可以在700-1000℃环境下长期使用。Compared with ordinary refractory fiber cotton and felt, the high-temperature-resistant flexible elastic gasket in the present disclosure has superior properties such as high strength, uniform thickness, and good continuity. It can withstand the axial vibration caused by pulse back blowing and dust removal. The thermal stress between the buffer ceramic film and the steel plate provides reliable fixed connection and sealing performance, and also has the advantages of simple manufacturing process and low cost. More importantly, the types of composite products have various forms, which can be made into various shapes, sizes, thicknesses, etc., with low thermal conductivity, non-combustion, high strength-to-weight ratio, good chemical stability, and good retention at high temperatures. Flexibility and other characteristics. The high-temperature-resistant flexible elastic gasket provided by the present disclosure can be used for a long time in an environment of 700-1000 ° C.
以下作为本公开优选的技术方案,但不作为对本公开提供的技术方案的限制,通过以下优选的技术方案,可以更好的达到和实现本公开的技术目的和有益效果。The following is a preferred technical solution of the present disclosure, but is not a limitation on the technical solution provided by the present disclosure. Through the following preferred technical solutions, the technical objectives and beneficial effects of the present disclosure can be better achieved and realized.
本公开中,以耐火纤维布作为密封垫的基材。In the present disclosure, a refractory fiber cloth is used as a base material of a gasket.
作为本公开优选的技术方案,所述密封垫中,耐火纤维布包括高硅氧纤维布、石英纤维布或硅酸铝纤维布中的任意一种或至少两种的组合。所述高硅氧纤维布是高纯氧化硅非晶体连续纤维布的简称,其氧化硅含量为96-98%。As a preferred technical solution of the present disclosure, in the gasket, the refractory fiber cloth includes any one or a combination of at least two of high-silica fiber cloth, quartz fiber cloth, or aluminum silicate fiber cloth. The high-silica fiber cloth is an abbreviation of high-purity silicon oxide amorphous continuous fiber cloth, and its silicon oxide content is 96-98%.
优选地,所述密封垫中,耐火纤维布的编织方式包括但不限于平纹、斜纹或缎面中的任意一种或至少两种的组合。但并不仅限于上述列举的编织方式,其他可达到相同效果的本领域常见编织方式也可用于本公开中。Preferably, in the sealing pad, the weaving manner of the refractory fiber cloth includes, but is not limited to, any one or a combination of at least two of plain weave, twill weave, or satin. However, it is not limited to the above-mentioned weaving methods, and other common weaving methods in the art that can achieve the same effect can also be used in the present disclosure.
作为本公开优选的技术方案,所述密封垫中,结合剂浆料以重量份计包括以下组分:As a preferred technical solution of the present disclosure, in the gasket, the binder slurry includes the following components in parts by weight:
Figure PCTCN2018091743-appb-000003
Figure PCTCN2018091743-appb-000003
Figure PCTCN2018091743-appb-000004
Figure PCTCN2018091743-appb-000004
优选的,所述密封垫中,结合剂浆料以重量份计包括以下组分:Preferably, in the sealing pad, the binder slurry includes the following components in parts by weight:
优选地,所述填料包括蛭石颗粒、莫来石短纤维或氧化锆短纤维中任意一种或至少两种的组合。典型但是非限制性的组合有:蛭石颗粒和莫来石短纤维的组合,莫来石短纤维和氧化锆短纤维的组合,蛭石颗粒和氧化锆短纤维的组合,蛭石颗粒、莫来石短纤维和氧化锆短纤维的组合。本公开中,所述短纤维的长度为100-500μm。Preferably, the filler comprises any one or a combination of at least two of vermiculite particles, mullite short fibers, or zirconia short fibers. Typical but non-limiting combinations are: a combination of vermiculite particles and mullite short fibers, a combination of mullite short fibers and zirconia short fibers, a combination of vermiculite particles and zirconia short fibers, vermiculite particles, A combination of short stone fibers and short zirconia fibers. In the present disclosure, the length of the short fibers is 100-500 μm.
本公开添加蛭石颗粒,通过弥散分布,能够有效地增加材料的耐温性能,扩大了密封垫的使用温度范围;本公开添加莫来石短纤维、氧化锆短纤维,通过随机排布,方向各异地分散在纤维布层间,起到一定支撑作用,以提高材料的回弹性。The present disclosure adds vermiculite particles, which can effectively increase the temperature resistance performance of the material and extend the use temperature range of the gasket through the dispersion distribution. The present disclosure adds mullite short fibers and zirconia short fibers. They are scattered in different layers between the fiber cloth layers to play a supporting role to improve the resilience of the material.
优选的,所述分散剂包括十二烷基苯磺酸盐、烷基二苯醚单磺酸盐、烷基二苯醚双磺酸盐、醇醚磺酸盐或酚醚磺酸盐中的任意一种或至少两种的组合。但并不仅限于上述分散剂,其他本领域可以达到同样效果的常见分散剂也可用于本公开,例如其他种类的阴离子表面活性剂。Preferably, the dispersant includes a dodecylbenzene sulfonate, an alkyl diphenyl ether monosulfonate, an alkyl diphenyl ether disulfonate, an alcohol ether sulfonate, or a phenol ether sulfonate. Any one or a combination of at least two. However, it is not limited to the above-mentioned dispersants, and other common dispersants that can achieve the same effect in the art can also be used in this disclosure, such as other types of anionic surfactants.
第二方面,本公开提供一种如第一方面所述密封垫的制备方法,所述方法包括以下步骤:In a second aspect, the present disclosure provides a method for preparing a gasket according to the first aspect, the method comprising the following steps:
(1)制备结合剂浆料;(1) preparing a binder slurry;
(2)将步骤(1)所得结合剂浆料复合在耐火纤维布需要粘合的面上,再对得到的复合了结合剂浆料的耐火纤维布进行叠加,最后加工成型,得到所述密封垫。(2) The binder slurry obtained in step (1) is compounded on the side of the refractory fiber cloth that needs to be bonded, and then the obtained refractory fiber cloth with the binder slurry is superimposed, and finally processed to form the seal. pad.
本公开提供的制备方法产品原料易得、环保,制备工艺简单,适于工业化应用,通过控制耐火纤维布的叠加层数即可控制厚度,通过控制加工成型模具即可控制形状。The preparation method provided by the present disclosure has readily available raw materials, environmental protection, simple preparation process, and is suitable for industrial application. The thickness can be controlled by controlling the number of layers of the refractory fiber cloth, and the shape can be controlled by controlling the processing and forming mold.
作为本公开优选的技术方案,步骤(1)中,所述制备结合剂浆料包括以下步骤:As a preferred technical solution of the present disclosure, in step (1), the preparation of the binder slurry includes the following steps:
将配比量的水性聚氨酯、环氧树脂乳液、铝溶胶和分散剂混合,得到混合乳液,再向所述混合乳液中加入配比量的填料,经分散后得到所述结合剂浆料。A proportion of a water-based polyurethane, an epoxy resin emulsion, an aluminum sol, and a dispersant are mixed to obtain a mixed emulsion, and a proportion of a filler is added to the mixed emulsion to obtain the binder slurry after dispersion.
作为本公开优选的技术方案,所述分散剂包括但不限于十二烷基苯磺酸盐、烷基二苯醚单磺酸盐、烷基二苯醚双磺酸盐、醇醚磺酸盐或酚醚磺酸盐中的任意一种或至少两种的组合。As a preferred technical solution of the present disclosure, the dispersant includes, but is not limited to, dodecylbenzenesulfonate, alkyldiphenyl ether monosulfonate, alkyldiphenyl ether disulfonate, and alcohol ether sulfonate Or any one or a combination of at least two of phenol ether sulfonates.
优选地,所述混合的方法包括搅拌。Preferably, the method of mixing comprises stirring.
优选地,所述填料包括蛭石颗粒、莫来石短纤维或氧化锆短纤维中任意一种或至少两种的组合。典型但是非限制性的组合有:蛭石颗粒和莫来石短纤维的组合,莫来石短纤维和氧化锆短纤维的组合,蛭石颗粒和氧化锆短纤维的组合,蛭石颗粒、莫来石短纤维和氧化锆短纤维的组合。本公开中,所述短纤维的长度为100-500μm。Preferably, the filler comprises any one or a combination of at least two of vermiculite particles, mullite short fibers, or zirconia short fibers. Typical but non-limiting combinations are: a combination of vermiculite particles and mullite short fibers, a combination of mullite short fibers and zirconia short fibers, a combination of vermiculite particles and zirconia short fibers, vermiculite particles, A combination of short stone fibers and short zirconia fibers. In the present disclosure, the length of the short fibers is 100-500 μm.
优选地,所述分散的方法包括超声分散、搅拌或球磨中的任意一种或至少两种的组合。典型但是非限制性的组合有:超声分散和搅拌的组合,搅拌和球磨的组合,超声分散和球磨的组合等。Preferably, the method of dispersion comprises any one or a combination of at least two of ultrasonic dispersion, stirring or ball milling. Typical but non-limiting combinations are: a combination of ultrasonic dispersion and stirring, a combination of stirring and ball milling, a combination of ultrasonic dispersion and ball milling, and the like.
作为本公开优选的技术方案,步骤(2)中,所述耐火纤维布包括高硅氧纤维布、石英纤维布或硅酸铝纤维布中的任意一种或至少两种的组合。所述高硅氧纤维布是高纯氧化硅非晶体连续纤维布的简称,其氧化硅含量为96-98%。As a preferred technical solution of the present disclosure, in step (2), the refractory fiber cloth includes any one or a combination of at least two of high-silica fiber cloth, quartz fiber cloth, or aluminum silicate fiber cloth. The high-silica fiber cloth is an abbreviation of high-purity silicon oxide amorphous continuous fiber cloth, and its silicon oxide content is 96-98%.
优选地,步骤(2)中,将步骤(1)所得结合剂浆料复合在耐火纤维布需要粘合的面上的方法为涂布或浸渍。Preferably, in the step (2), the method for compounding the binder slurry obtained in the step (1) on the surface to be bonded of the refractory fiber cloth is coating or dipping.
优选地,步骤(2)中,耐火纤维布需要粘合的面上复合的结合剂浆料的量为0.01~0.5g/cm 2,例如0.01g/cm 2、0.05g/cm 2、0.1g/cm 2、0.2g/cm 2、0.3g/cm 2、0.4g/cm 2或0.5g/cm 2等,但并不仅限于所列举的数值,该数值范围内其他未列举的数值同样适用。 Preferably, in the step (2), the amount of the binder slurry compounded on the surface to be bonded of the refractory fiber cloth is 0.01 to 0.5 g / cm 2 , for example, 0.01 g / cm 2 , 0.05 g / cm 2 , 0.1 g / cm 2, 0.2g / cm 2 , 0.3g / cm 2, 0.4g / cm 2 or 0.5g / cm 2 and the like, but are not limited to the exemplified values, other unrecited number within the numerical range applies.
优选地,步骤(2)中,所述叠加的方法为将复合了结合剂浆料的耐火纤维布多层叠加之后再加压烘干或将复合了结合剂浆料的耐火纤维布单层烘干之后再多层加压叠加。本公开中,所述多层是指≥2层。Preferably, in step (2), the superimposing method is to laminate the refractory fiber cloth compounded with the binder slurry in multiple layers and then press-dry it or bake the refractory fiber cloth compounded with the binder slurry in a single layer. After drying, multiple layers of pressure are stacked. In the present disclosure, the multilayer refers to ≥ 2 layers.
优选地,所述加压的压力为1~10MPa,例如1MPa、2MPa、3MPa、4MPa、5MPa、6MPa、7MPa、8MPa、9MPa或10MPa等,但并不仅限于所列举的数值,该数值范围内其他未列举的数值同样适用。Preferably, the pressing pressure is 1 to 10 MPa, for example, 1 MPa, 2 MPa, 3 MPa, 4 MPa, 5 MPa, 6 MPa, 7 MPa, 8 MPa, 9 MPa, or 10 MPa, etc., but is not limited to the listed values. Unlisted values also apply.
优选地,步骤(2)中,所述加工成型的方法为模切成型。Preferably, in step (2), the method of processing and forming is die cutting.
作为本公开优选的技术方案,步骤(2)中,所述耐火纤维布在经过预处理后再与结合剂浆料复合。As a preferred technical solution of the present disclosure, in step (2), the refractory fiber cloth is compounded with a binder slurry after pretreatment.
优选地,所述预处理为脱浆处理。Preferably, the pretreatment is a desizing treatment.
优选地,所述脱浆处理的方法包括在乙醇中超声震荡后烘干和/或600℃加热。本公开中,所述在乙醇中超声震荡后烘干和/或600℃加热是指可以为在乙醇中超声震荡后烘干,也可以为600℃加热,还可以为在乙醇中超声震荡后烘干和600℃加热的组合。Preferably, the method for the desizing treatment includes drying and / or heating at 600 ° C. after ultrasonic vibration in ethanol. In the present disclosure, the drying after ultrasonic vibration in ethanol and / or heating at 600 ° C. means that drying may be performed after ultrasonic vibration in ethanol, heating may be performed at 600 ° C., or drying after ultrasonic vibration in ethanol may be used. A combination of dry and 600 ° C heating.
作为本公开所述制备方法的进一步优选技术方案,所述方法包括以下步骤:As a further preferred technical solution of the preparation method according to the present disclosure, the method includes the following steps:
(1)将配比量的水性聚氨酯、环氧树脂乳液、铝溶胶和分散剂搅拌混合,得到混合乳液,再向所述混合乳液中加入配比量的填料,经分散后得到所述结合剂浆料;(1) Mixing a proportion of a water-based polyurethane, an epoxy resin emulsion, an aluminum sol, and a dispersant to obtain a mixed emulsion, and adding a proportion of a filler to the mixed emulsion to obtain the binding agent after dispersion. Slurry
(2)将步骤(1)所得结合剂浆料用涂布或浸渍的方法复合在脱浆处理过的耐火纤维布需要粘合的面上,再对得到的复合了结合剂浆料的耐火纤维布进行叠加,最后模切成型,得到所述密封垫;(2) Compounding the binder slurry obtained in step (1) by coating or impregnating it on the surface of the desizing-treated refractory fiber cloth to be bonded, and then combining the obtained refractory fiber with the binder slurry The cloths are superimposed, and finally die-cut to obtain the sealing gasket;
其中,耐火纤维布需要粘合的面上复合的结合剂浆料的量为0.01~0.5g/cm 2,所述叠加的方法为将复合了结合剂浆料的耐火纤维布多层叠加之后再加压烘干或将复合了结合剂浆料的耐火纤维布单层烘干之后再多层加压叠加,所述加压的压力为1~10MPa。 The amount of the binder slurry compounded on the surface to be bonded of the refractory fiber cloth is 0.01 to 0.5 g / cm 2 , and the superimposing method is to stack the refractory fiber cloth compounded with the binder slurry in multiple layers, and then Pressure drying or single-layer drying of the refractory fiber cloth combined with the binder slurry is followed by multiple layers of pressure stacking, and the pressing pressure is 1 to 10 MPa.
第三方面,本公开提供一种如第一方面所述密封垫的用途,所述密封垫用于密封刚性异质管件间的连接处。本公开提供的密封垫可以用于石油化工、冶金、建材、电力等高温管件连接场合,尤其适用于陶瓷膜和钢板的接触密封面,可以对高温下连接处管件的膨胀起到很好地缓冲作用,且密封效果良好。In a third aspect, the present disclosure provides the use of the gasket according to the first aspect, which is used to seal a connection between rigid heterogeneous pipe fittings. The gasket provided by the present disclosure can be used in the connection of high temperature pipe fittings such as petrochemical industry, metallurgy, building materials, electricity, etc., and is particularly suitable for the contact sealing surface of ceramic film and steel plate, which can well buffer the expansion of the pipe fittings at high temperature Effect and good sealing effect.
与现有技术相比,本公开具有以下有益效果:Compared with the prior art, the present disclosure has the following beneficial effects:
(1)本公开通过将水性聚氨酯、环氧树脂乳液、填料、铝溶胶、分散剂混合,形成结合剂浆料,在保证粘性和环保性的同时,有效地提高了密封垫的机械强度,常温下强度高、不硬化,高温下柔性好、不脆断,能更好地满足材料的高温柔弹性;(1) The present disclosure forms a binder slurry by mixing water-based polyurethane, epoxy resin emulsion, filler, aluminum sol, and dispersant, which effectively improves the mechanical strength of the gasket, while ensuring viscosity and environmental protection, at room temperature. High strength, no hardening, good flexibility at high temperature, no brittle fracture, can better meet the high temperature flexibility of the material;
(2)本公开通过耐火纤维布的多层复合,使材料具有高机械强度,同时,多层纤维可在压力和热应力下自调适所受到的刚性点应力,通过缝隙补偿及优良的抗腐蚀性,提高材料的密封性能;(2) The present disclosure makes the material have high mechanical strength through multilayer composite of refractory fiber cloth. At the same time, the multilayer fiber can self-adjust the rigid point stress it receives under pressure and thermal stress, through gap compensation and excellent corrosion resistance And improve the sealing performance of the material;
(3)本公开添加蛭石颗粒,通过弥散分布,能够有效地增加材料的耐温性能,扩大了密封垫的使用温度范围;(3) The addition of vermiculite particles in the present disclosure can effectively increase the temperature resistance of the material through the dispersion distribution, and expand the use temperature range of the gasket;
(4)本公开添加莫来石短纤维、氧化锆短纤维,通过随机排布,方向各异地分散在纤维布层间,起到一定支撑作用,以提高材料的回弹性;(4) The mullite short fibers and zirconia short fibers are added in the present disclosure, and are randomly dispersed in different directions between the fiber cloth layers to play a supporting role to improve the resilience of the material;
(5)本公开提供的耐高温的柔弹性密封垫可以在700-1000℃环境下长期使用,具有与密封面结合紧密的柔弹性,为面密封且密封面较大,因此密封效果好,对刚性异质管件连接处起到柔性密封和缓冲作用,整体性好,不粘附在管件表面上,可清理,拆装更换便捷;(5) The high-temperature-resistant, flexible and elastic gasket provided in this disclosure can be used for a long time in an environment of 700-1000 ° C, and has a flexible elasticity that is tightly combined with the sealing surface. The joints of rigid and heterogeneous pipe fittings play the role of flexible sealing and cushioning, have good integrity, do not stick to the surface of the pipe fittings, can be cleaned, and are easy to disassemble and replace;
(6)本公开提供的耐高温的柔弹性密封垫原料易得、环保,制备工艺简单,适于工业化应用。(6) The high-temperature-resistant flexible elastic gaskets provided in the present disclosure have readily available raw materials, are environmentally friendly, have simple preparation processes, and are suitable for industrial applications.
附图说明BRIEF DESCRIPTION OF THE DRAWINGS
图1为本公开实施例1制备的密封垫的截面(不限于此图所示叠加层数)示意图,其中1-耐火纤维布,2-结合剂浆料;FIG. 1 is a schematic cross-sectional view (not limited to the number of superimposed layers) of the gasket prepared in Example 1 of the present disclosure, where 1-refractory fiber cloth, 2-binder slurry;
图2为本公开实施例1制备的O形环状密封垫的整体结构示意图。FIG. 2 is a schematic diagram of the overall structure of an O-ring seal prepared in Example 1 of the present disclosure.
具体实施方式Detailed ways
为更好地说明本公开,便于理解本公开的技术方案,下面对本公开进一步详细说明。但下述的实施例仅仅是本公开的简易例子,并不代表或限制本公开的权利保护范围,本公开保护范围以权利要求书为准。In order to better explain the present disclosure and facilitate understanding of the technical solutions of the present disclosure, the present disclosure is further described in detail below. However, the following embodiments are merely simple examples of the present disclosure, and do not represent or limit the scope of protection of the rights of the present disclosure. The scope of protection of the present disclosure is subject to the claims.
以下为本公开典型但非限制性实施例:The following are typical but non-limiting examples of this disclosure:
实施例1Example 1
按以下步骤制备密封垫:Prepare the gasket as follows:
本实施例中密封垫的结合剂浆料的组分及配比选择为:52份的水性聚氨酯、30份的环氧树脂乳液、13份的填料、5份的铝溶胶,外加0.8份的分散剂。In this embodiment, the components and ratio of the binder slurry of the gasket are selected as: 52 parts of water-based polyurethane, 30 parts of epoxy resin emulsion, 13 parts of filler, 5 parts of aluminum sol, and 0.8 part of dispersion Agent.
(1)将水性聚氨酯、环氧树脂乳液、铝溶胶和分散剂加入高速混合机搅拌20min,充分混合均匀后,加入13份的填料。填料的组成为蛭石颗粒和莫来石短纤维按1 1的质量比例添加。球磨1h后形成稳定的结合剂浆料。所述分散剂为十二烷基苯磺酸钠。 (1) Add water-based polyurethane, epoxy resin emulsion, aluminum sol, and dispersant to a high-speed mixer for 20 minutes, mix thoroughly, and then add 13 parts of filler. The composition of the filler is vermiculite particles and mullite short fibers added at a mass ratio of 1 : 1. A stable binder slurry was formed after ball milling for 1 h. The dispersant is sodium dodecylbenzenesulfonate.
(2)使用纯度高于96%的平纹高硅氧纤维布作为基材,经600℃高温预处理30min后,使用自动滚胶机将结合剂浆料均匀涂布在纤维布上下两面,涂布量约为0.1g/cm 2,经70℃红外线烘干1h,散失大量水分后,多层叠加,在10MPa压力下复合成型。最后,通过模切,即获得内直径7cm、外直径9cm的O形耐高温柔弹性密封垫。 (2) Using plain weave high-silicone fiber cloth with a purity higher than 96% as the substrate, and after high-temperature pretreatment at 600 ° C for 30 minutes, the adhesive slurry is evenly coated on the upper and lower sides of the fiber cloth using an automatic tumbling machine to coat The amount is about 0.1g / cm 2. After infrared drying at 70 ° C. for 1 hour, a large amount of water is lost, and then the layers are superimposed and compounded under a pressure of 10 MPa. Finally, through die cutting, an O-shaped high-temperature-resistant flexible elastic gasket with an inner diameter of 7 cm and an outer diameter of 9 cm is obtained.
本实施例制备的密封垫可用于高温陶瓷膜过滤管的密封,安装在多孔钢板和陶瓷过滤管之间,在陶瓷管顶部压紧作用力下,密封垫受到挤压发生弹性形变,从而填充高温陶瓷管与多孔钢板之间的间隙,达到有效密封的效果。The gasket prepared in this embodiment can be used for sealing high-temperature ceramic membrane filter tubes. It is installed between the porous steel plate and the ceramic filter tube. Under the pressing force of the top of the ceramic tube, the gasket is elastically deformed by compression, thereby filling the high temperature. The gap between the ceramic tube and the porous steel plate achieves an effective sealing effect.
本实施例制备的密封垫的截面如图1所示(不限于此图所示叠加层数),密封垫由耐火纤维布1和结合剂浆料2组成,所述耐火纤维布1相互叠加,所述结合剂浆料2位于相邻的耐火纤维布1之间以及最外层耐火纤维布1的外侧面。The cross section of the gasket prepared in this embodiment is shown in FIG. 1 (not limited to the number of superimposed layers shown in this figure). The gasket is composed of a refractory fiber cloth 1 and a binder slurry 2. The refractory fiber cloth 1 is superimposed on each other. The binder slurry 2 is located between adjacent refractory fiber cloths 1 and the outer side of the outermost refractory fiber cloth 1.
本实施例制备的密封垫的整体结构示意图如图2所示,为O形环状。A schematic diagram of the overall structure of the gasket prepared in this embodiment is shown in FIG. 2 and is an O-ring.
测试结果表明,本实施例制备的密封垫具有与密封面紧密结合的柔软性,起到柔弹性密封和缓冲应力作用,可以在700-1000℃环境下长期使用。经过长时间耐温测试,发现其在高温下的密封效果好、整体性及强度高,不粘附在管件表面上,可快速清理,拆装更换便捷。可以用于高温烟气净化的陶瓷膜过滤管密封,如钢厂烟气净化等工业高温烟气净化设备。The test results show that the gasket prepared in this embodiment has the flexibility of tightly combining with the sealing surface, plays a role of flexible elastic sealing and buffering stress, and can be used for a long time in an environment of 700-1000 ° C. After a long-term temperature resistance test, it was found that it has a good sealing effect, high integrity and high strength at high temperatures, does not adhere to the surface of the pipe, can be quickly cleaned, and is easy to disassemble and replace. Ceramic membrane filter tubes that can be used for high temperature flue gas purification, such as steel plant flue gas purification and other industrial high temperature flue gas purification equipment.
本实施例制备的五层叠加的密封垫长期在1000℃下使用,抗拉强度保持在35.9MPa左右。The five-layer superimposed gasket prepared in this embodiment is used at 1000 ° C. for a long time, and the tensile strength is maintained at about 35.9 MPa.
实施例2Example 2
按以下步骤制备耐高温的柔弹性密封垫:Follow these steps to prepare a heat-resistant, flexible and elastic gasket:
本实施例中密封材料的结合剂浆料组分及配比选择为:68份的水性聚氨酯、16份的环氧树脂乳液、15份的填料、1份的铝溶胶,外加1份的分散剂。In this embodiment, the binder slurry component and the mixing ratio of the sealing material are selected as: 68 parts of water-based polyurethane, 16 parts of epoxy resin emulsion, 15 parts of filler, 1 part of aluminum sol, and 1 part of dispersant. .
(1)将水性聚氨酯、环氧树脂乳液、铝溶胶和分散剂加入高速混合机搅拌20min,混合均匀后,加入15份的填料。填料的组成为蛭石颗粒、莫来石短纤维和氧化锆短纤维按2∶1∶1的质量比例添加。搅拌后形成稳定的结合剂浆料。所述搅拌速度控制在800转/min,搅拌50min。所述分散剂为烷基二苯醚单磺酸钠。(1) Add water-based polyurethane, epoxy resin emulsion, aluminum sol, and dispersant into a high-speed mixer and stir for 20 minutes. After mixing, add 15 parts of filler. The composition of the filler is vermiculite particles, mullite short fibers and zirconia short fibers added at a mass ratio of 2: 1: 1. After stirring, a stable binder slurry was formed. The stirring speed was controlled at 800 rpm and stirred for 50 minutes. The dispersant is sodium alkyl diphenyl ether monosulfonate.
(2)使用纯度高于96%的缎面高硅氧纤维布作为基材,经乙醇超声震荡、烘干及600℃高温预处理后,使用刮胶器将结合剂浆料均匀平整涂布于纤维布上下两面,涂布量约为0.3g/cm 2,按布面纹理相同的面进行多层叠加,在1MPa压力下,50℃烘干10h。最后,通过模切即得到耐高温柔弹性密封垫。 (2) Using a satin high-silicone fiber cloth with a purity higher than 96% as a substrate, and after ultrasonic vibration of ethanol, drying and high-temperature pretreatment at 600 ° C, the adhesive slurry is evenly and evenly coated with a doctor blade. The upper and lower sides of the fiber cloth are coated with an amount of about 0.3 g / cm 2. Multi-layer superposition is performed according to the same surface of the cloth texture, and dried at 50 ° C. for 10 hours under a pressure of 1 MPa. Finally, a high-temperature-resistant flexible elastic gasket is obtained by die cutting.
本实施例制备的密封垫的截面参照实施例1(具体叠加层数不限于实施例1的层数),密封垫由耐火纤维布1和结合剂浆料2组成,所述耐火纤维布1相互叠加,所述结合剂浆料2位于相邻的耐火纤维布1之间以及最外层耐火纤维布1的外侧面。The cross section of the gasket prepared in this embodiment refers to Example 1 (the specific number of layers is not limited to the number of layers in Example 1). The gasket is composed of a refractory fiber cloth 1 and a binder slurry 2. Superposed, the binder slurry 2 is located between adjacent refractory fiber cloths 1 and the outer side of the outermost refractory fiber cloth 1.
测试结果表明,本实施例制备的密封垫具有与密封面紧密结合的柔软性,起到柔弹性密封和缓冲应力作用,可以在700-1000℃环境下长期使用。经过长时间耐温测试,发现其在高温下的密封效果好、整体性及强度高,不粘附在管件表面上,可快速清理,拆装更换便捷。可以用于高温烟气净化的陶瓷膜过滤管密封,如钢厂烟气净化等工业高温烟气净化设备。The test results show that the gasket prepared in this embodiment has the flexibility of tightly combining with the sealing surface, plays a role of flexible elastic sealing and buffering stress, and can be used for a long time in an environment of 700-1000 ° C. After a long-term temperature resistance test, it was found that it has a good sealing effect, high integrity and high strength at high temperatures, does not adhere to the surface of the pipe, can be quickly cleaned, and is easy to disassemble and replace. Ceramic membrane filter tubes that can be used for high temperature flue gas purification, such as steel plant flue gas purification and other industrial high temperature flue gas purification equipment.
本实施例制备的五层叠加的密封垫在1000℃下连续使用20h,抗拉强度保持在25.2MPa左右,强度不下降。The five-layer stacked gasket prepared in this embodiment is used continuously at 1000 ° C. for 20 hours, and the tensile strength is maintained at about 25.2 MPa, and the strength does not decrease.
实施例3Example 3
按以下步骤制备耐高温的柔弹性密封垫:Follow these steps to prepare a heat-resistant, flexible and elastic gasket:
本实施例中高温密封垫的结合剂浆料组分及配比选择为:65份的水性聚氨酯、22份的环氧树脂乳液、10份的填料、3份的铝溶胶,外加0.5份的分散剂。In this embodiment, the binder slurry components and mixing ratio of the high-temperature gasket are selected as follows: 65 parts of water-based polyurethane, 22 parts of epoxy resin emulsion, 10 parts of filler, 3 parts of aluminum sol, and 0.5 part of dispersion Agent.
(1)将水性聚氨酯、环氧树脂乳液、铝溶胶和分散剂加入高速混合机搅拌50min,搅拌均匀后,加入10份的填料。填料的组成为蛭石颗粒和莫来石短纤维按2∶1的质量比例添加。混合后形成稳定的结合剂浆料。所述分散剂为十二烷基苯磺酸钠。(1) Add water-based polyurethane, epoxy resin emulsion, aluminum sol, and dispersant to a high-speed mixer for 50 minutes. After stirring, add 10 parts of filler. The composition of the filler is that vermiculite particles and mullite short fibers are added in a mass ratio of 2: 1. After mixing, a stable binder slurry is formed. The dispersant is sodium dodecylbenzenesulfonate.
(2)使用不锈钢丝增强的平纹硅酸铝纤维布作为基材,将纤维布浸渍于上述浆料后,三层叠加,在2MPa压力下,60℃烘干5h。最后,通过模切即得到耐高温柔弹性密封垫。(2) Using stainless steel wire-reinforced plain-grain aluminum silicate fiber cloth as a base material, the fiber cloth was immersed in the above slurry, and then three layers were stacked, and dried at 60 ° C. for 5 hours under a pressure of 2 MPa. Finally, a high-temperature-resistant flexible elastic gasket is obtained by die cutting.
本实施例制备的密封垫的截面参照实施例1(具体叠加层数不限于实施例1的层数),密封垫由耐火纤维布1和结合剂浆料2组成,所述耐火纤维布1相互叠加,所述结合剂浆料2位于相邻的耐火纤维布1之间以及最外层耐火纤维布1的外侧面。The cross section of the gasket prepared in this embodiment refers to Example 1 (the specific number of layers is not limited to the number of layers in Example 1). The gasket is composed of a refractory fiber cloth 1 and a binder slurry 2. The refractory fiber cloth 1 is mutually Superposed, the binder slurry 2 is located between adjacent refractory fiber cloths 1 and the outer side of the outermost refractory fiber cloth 1.
测试结果表明,本实施例制备的密封垫具有与密封面紧密结合的柔软性,起到柔弹性密封和缓冲应力作用,可以在700℃环境下长期使用。经过长时间耐温测试,发现其在高温下的密封效果好、整体性及强度高,不粘附在管件表面上,可快速清理,拆装更换便捷。可以用于高温烟气净化的陶瓷膜过滤管密封,如钢厂烟气净化等工业高温烟气净化设备。The test results show that the gasket prepared in this embodiment has the flexibility of tightly combining with the sealing surface, plays a role of flexible elastic sealing and buffering stress, and can be used for a long time in an environment of 700 ° C. After a long-term temperature resistance test, it was found that it has a good sealing effect, high integrity and high strength at high temperatures, does not adhere to the surface of the pipe, can be quickly cleaned, and is easy to disassemble and replace. Ceramic membrane filter tubes that can be used for high temperature flue gas purification, such as steel plant flue gas purification and other industrial high temperature flue gas purification equipment.
本实施例制备的三层叠加的密封垫在700℃下长时间使用,抗拉强度保持在27.5MPa左右。The three-layer stacked gasket prepared in this embodiment is used at 700 ° C. for a long time, and the tensile strength is maintained at about 27.5 MPa.
实施例4Example 4
本实施例的具体步骤参照实施例1,区别在于,密封垫的结合剂浆料的组分中,水性聚氨酯的重量份数为50份,环氧树脂乳液的重量份数为35份;步骤(2)中,涂布量约为0.01g/cm 2The specific steps of this embodiment refer to Example 1. The difference is that among the components of the binder slurry of the gasket, 50 parts by weight of the aqueous polyurethane and 35 parts by weight of the epoxy resin emulsion; In 2), the coating amount was about 0.01 g / cm 2 .
本实施例制备的密封垫的截面参照实施例1(具体叠加层数不限于实施例1的层数),密封垫由耐火纤维布1和结合剂浆料2组成,所述耐火纤维布1相互叠加,所述结合剂浆料2位于相邻的耐火纤维布1之间以及最外层耐火纤维布1的外侧面。The cross section of the gasket prepared in this embodiment refers to Example 1 (the specific number of layers is not limited to the number of layers in Example 1). The gasket is composed of a refractory fiber cloth 1 and a binder slurry 2. The refractory fiber cloth 1 is mutually Superposed, the binder slurry 2 is located between adjacent refractory fiber cloths 1 and the outer side of the outermost refractory fiber cloth 1.
测试结果表明,本实施例制备的密封垫具有与密封面紧密结合的柔软性,起到柔弹性密封和缓冲应力作用,可以在700-1000℃环境下长期使用。经过长时间耐温测试,发现其在高温下的密封效果好、整体性及强度高,不粘附在管件表面上,可快速清理,拆装更换便捷。可以用于高温烟气净化的陶瓷膜过滤管密封,如钢厂烟气净化等工业高温烟气净化设备。The test results show that the gasket prepared in this embodiment has the flexibility of tightly combining with the sealing surface, plays a role of flexible elastic sealing and buffering stress, and can be used for a long time in an environment of 700-1000 ° C. After a long-term temperature resistance test, it was found that it has a good sealing effect, high integrity and high strength at high temperatures, does not adhere to the surface of the pipe, can be quickly cleaned, and is easy to disassemble and replace. Ceramic membrane filter tubes that can be used for high temperature flue gas purification, such as steel plant flue gas purification and other industrial high temperature flue gas purification equipment.
本实施例制备的五层叠加的密封垫长期900℃下使用,抗拉强度保持在38.8MPa左右。The five-layer stacked gasket prepared in this embodiment is used at 900 ° C. for a long time, and the tensile strength is maintained at about 38.8 MPa.
实施例5Example 5
本实施例的具体步骤参照实施例1,区别在于,密封垫的结合剂浆料的组分中,水性聚氨酯的重量份数为70份,环氧树脂乳液的重量份数为10份;步骤(2)中,涂布量约为0.5g/cm 2The specific steps of this embodiment refer to Example 1. The difference is that among the components of the binder slurry of the gasket, 70 parts by weight of the aqueous polyurethane and 10 parts by weight of the epoxy resin emulsion; steps ( In 2), the coating amount was about 0.5 g / cm 2 .
本实施例制备的密封垫的截面参照实施例1(具体叠加层数不限于实施例1的层数),密封垫由耐火纤维布1和结合剂浆料2组成,所述耐火纤维布1相互叠加,所述结合剂浆料2位于相邻的耐火纤维布1之间以及最外层耐火纤维布1的外侧面。The cross section of the gasket prepared in this embodiment refers to Example 1 (the specific number of layers is not limited to the number of layers in Example 1). The gasket is composed of a refractory fiber cloth 1 and a binder slurry 2. The refractory fiber cloth 1 is mutually Superposed, the binder slurry 2 is located between adjacent refractory fiber cloths 1 and the outer side of the outermost refractory fiber cloth 1.
测试结果表明,本实施例制备的密封垫具有与密封面紧密结合的柔软性, 起到柔弹性密封和缓冲应力作用,可以在700-1000℃环境下长期使用。经过长时间耐温测试,发现其在高温下的密封效果好、整体性及强度高,不粘附在管件表面上,可快速清理,拆装更换便捷。可以用于高温烟气净化的陶瓷膜过滤管密封,如钢厂烟气净化等工业高温烟气净化设备。The test results show that the gasket prepared in this embodiment has the flexibility of tightly combining with the sealing surface, plays a role of flexible elastic sealing and buffering stress, and can be used for a long time in an environment of 700-1000 ° C. After a long-term temperature resistance test, it was found that it has a good sealing effect, high integrity and high strength at high temperatures, does not adhere to the surface of the pipe, can be quickly cleaned, and is easy to disassemble and replace. Ceramic membrane filter tubes that can be used for high temperature flue gas purification, such as steel plant flue gas purification and other industrial high temperature flue gas purification equipment.
本实施例制备的五层叠加的密封垫长期1000℃下使用,抗拉强度保持在34.3MPa左右。The five-layer stacked gasket prepared in this embodiment is used at 1000 ° C. for a long time, and the tensile strength is maintained at about 34.3 MPa.
对比例1Comparative Example 1
本对比例的具体步骤参照实施例1,区别在于,结合剂浆料中不加入填料。The specific steps of this comparative example refer to Example 1, with the difference that no filler is added to the binder slurry.
本对比例的结果为制备出的密封垫因为不添加填料,浆料粘度较小,多层叠加后烘干时间较长,且容易造成材料边缘水分散失速度较材料中部水分散失速度差异较大,导致材料收缩不均,平整度下降等不良后果。The result of this comparative example is that the prepared gasket has a small viscosity due to the absence of fillers, a long drying time after multi-layer superposition, and the water dispersion loss rate at the edge of the material is likely to be significantly different from the water dispersion loss rate at the middle of the material. Lead to adverse consequences such as uneven shrinkage of the material and reduction in flatness.
综合上述实施例和对比例可知,本公开提供的密封垫具有耐高温、柔韧性强的特点,经过多层复合,可以获得厚度可控,形状可塑的立体密封材料,起到刚性异质管件连接处的柔性密封作用。同时,还具有制作工艺简单,能耗低的特点,可以用于石油化工、冶金、建材、电力等高温管件连接场合。对比例没有采用本公开的方案,因而无法取得本公开的效果。Based on the above embodiments and comparative examples, it can be seen that the gasket provided by the present disclosure has the characteristics of high temperature resistance and strong flexibility. After multilayer composite, a three-dimensional sealing material with a controllable thickness and a plastic shape can be obtained, and the rigid heterogeneous pipe connection can be achieved. Flexible sealing effect. At the same time, it also has the characteristics of simple manufacturing process and low energy consumption, which can be used in the connection of high temperature pipe fittings such as petrochemical, metallurgy, building materials, and power. The comparative example did not adopt the scheme of the present disclosure, so the effects of the present disclosure could not be obtained.
申请人声明,以上所述仅为本发明的具体实施方式,但本发明的保护范围并不局限于此,所属技术领域的技术人员应该明了,任何属于本技术领域的技术人员在本公开揭露的技术范围内,可轻易想到的变化或替换,均落在本发明的保护范围和公开范围之内。The applicant states that the above description is only a specific embodiment of the present invention, but the scope of protection of the present invention is not limited to this. Those skilled in the art should understand that any person disclosed in this disclosure by those skilled in the art Within the technical scope, changes or replacements that can be easily conceived all fall within the scope of protection and disclosure of the present invention.

Claims (11)

  1. 一种密封垫,其包括耐火纤维布(1)和结合剂浆料(2),所述耐火纤维布(1)相互叠加,所述结合剂浆料(2)位于相邻的耐火纤维布(1)之间以及最外层耐火纤维布(1)的外侧面;A gasket comprises a refractory fiber cloth (1) and a binder slurry (2), the refractory fiber cloth (1) is superimposed on each other, and the binder slurry (2) is located in an adjacent refractory fiber cloth ( 1) between and the outer side of the outermost layer of refractory fiber cloth (1);
    所述结合剂浆料(2)以重量份计包括以下组分:The binder slurry (2) includes the following components in parts by weight:
    Figure PCTCN2018091743-appb-100001
    Figure PCTCN2018091743-appb-100001
  2. 根据权利要求1所述的密封垫,其中,所述密封垫中,耐火纤维布(1)包括高硅氧纤维布、石英纤维布或硅酸铝纤维布中的任意一种或至少两种的组合。The gasket according to claim 1, wherein in the gasket, the refractory fiber cloth (1) includes any one or at least two of high-silica fiber cloth, quartz fiber cloth, or aluminum silicate fiber cloth combination.
  3. 根据权利要求1或2所述的密封垫,其中,所述密封垫中,耐火纤维布(1)的编织方式包括平纹、斜纹或缎面中的任意一种或至少两种的组合。The gasket according to claim 1 or 2, wherein the weaving manner of the refractory fiber cloth (1) in the gasket comprises any one of plain weave, twill weave, or satin, or a combination of at least two of them.
  4. 根据权利要求1-3任一项所述的密封垫,其中,所述密封垫中,结合剂浆料(2)以重量份计包括以下组分:The gasket according to any one of claims 1-3, wherein in the gasket, the binder slurry (2) includes the following components in parts by weight:
    Figure PCTCN2018091743-appb-100002
    Figure PCTCN2018091743-appb-100002
    优选的,所述密封垫中,结合剂浆料(2)以重量份计包括以下组分:Preferably, in the gasket, the binder slurry (2) includes the following components in parts by weight:
    Figure PCTCN2018091743-appb-100003
    Figure PCTCN2018091743-appb-100003
    Figure PCTCN2018091743-appb-100004
    Figure PCTCN2018091743-appb-100004
    优选地,所述填料包括蛭石颗粒、莫来石短纤维或氧化锆短纤维中任意一种或至少两种的组合;Preferably, the filler comprises any one or a combination of at least two of vermiculite particles, mullite short fibers, or zirconia short fibers;
    优选的,所述分散剂包括十二烷基苯磺酸盐、烷基二苯醚单磺酸盐、烷基二苯醚双磺酸盐、醇醚磺酸盐或酚醚磺酸盐中的任意一种或至少两种的组合。Preferably, the dispersant includes a dodecylbenzene sulfonate, an alkyl diphenyl ether monosulfonate, an alkyl diphenyl ether disulfonate, an alcohol ether sulfonate, or a phenol ether sulfonate. Any one or a combination of at least two.
  5. 如权利要求1-4任一项所述的密封垫的制备方法,其包括以下步骤:The method for preparing a gasket according to any one of claims 1-4, comprising the following steps:
    (1)制备结合剂浆料(2);(1) preparing a binder slurry (2);
    (2)将步骤(1)所得结合剂浆料(2)复合在耐火纤维布(1)需要粘合的面上,再对得到的复合了结合剂浆料(2)的耐火纤维布(1)进行叠加,最后加工成型,得到所述密封垫。(2) The binder slurry (2) obtained in step (1) is compounded on the surface of the refractory fiber cloth (1) to be bonded, and the obtained refractory fiber cloth (1) compounded with the binder slurry (2) is further compounded. ) Superimposing, and finally processing and forming, to obtain the sealing gasket.
  6. 根据权利要求5所述的制备方法,其中,步骤(1)中,所述制备结合剂浆料(2)包括以下步骤:The method according to claim 5, wherein in step (1), the step of preparing the binder slurry (2) comprises the following steps:
    将配比量的水性聚氨酯、环氧树脂乳液、铝溶胶和分散剂混合,得到混合乳液,再向所述混合乳液中加入配比量的填料,经分散后得到所述结合剂浆料(2)。A proportion of a water-based polyurethane, an epoxy resin emulsion, an aluminum sol, and a dispersant are mixed to obtain a mixed emulsion, and a proportion of a filler is added to the mixed emulsion to obtain the binder slurry (2) after dispersion. ).
  7. 根据权利要求6所述的制备方法,其中,所述分散剂包括十二烷基苯磺酸盐、烷基二苯醚单磺酸盐、烷基二苯醚双磺酸盐、醇醚磺酸盐或酚醚磺酸盐中的任意一种或至少两种的组合;The method according to claim 6, wherein the dispersant comprises dodecylbenzenesulfonate, alkyldiphenylether monosulfonate, alkyldiphenylether disulfonate, alcohol ethersulfonic acid Any one or a combination of at least two salts or phenol ether sulfonates;
    优选地,所述混合的方法包括搅拌;Preferably, the method of mixing includes stirring;
    优选地,所述填料包括蛭石颗粒、莫来石短纤维或氧化锆短纤维中任意一 种或至少两种的组合;Preferably, the filler comprises any one or a combination of at least two of vermiculite particles, mullite short fibers, or zirconia short fibers;
    优选地,所述分散的方法包括超声分散、搅拌或球磨中的任意一种或至少两种的组合。Preferably, the method of dispersion comprises any one or a combination of at least two of ultrasonic dispersion, stirring or ball milling.
  8. 根据权利要求5-7任一项所述的制备方法,其中,步骤(2)中所述耐火纤维布(1)包括高硅氧纤维布、石英纤维布或硅酸铝纤维布中的任意一种或至少两种的组合;The preparation method according to any one of claims 5 to 7, wherein the refractory fiber cloth (1) in step (2) comprises any one of a high-silica fiber cloth, a quartz fiber cloth, or an aluminum silicate fiber cloth Or a combination of at least two;
    优选地,步骤(2)中,将步骤(1)所得结合剂浆料(2)复合在耐火纤维布(1)需要粘合的面上的方法为涂布或浸渍;Preferably, in step (2), the method of compounding the binder slurry (2) obtained in step (1) on the surface of the refractory fiber cloth (1) to be bonded is coating or dipping;
    优选地,步骤(2)中,耐火纤维布(1)需要粘合的面上复合的结合剂浆料(2)的量为0.01~0.5g/cm 2Preferably, in the step (2), the amount of the binder slurry (2) compounded on the surface to be bonded of the refractory fiber cloth (1) is 0.01 to 0.5 g / cm 2 ;
    优选地,步骤(2)中,所述叠加的方法为将复合了结合剂浆料(2)的耐火纤维布(1)多层叠加之后再加压烘干或将复合了结合剂浆料(2)的耐火纤维布(1)单层烘干之后再多层加压叠加;Preferably, in step (2), the superimposing method is to laminate the refractory fiber cloth (1) compounded with the binder slurry (2) in multiple layers, and then pressurize and dry it, or compound the binder slurry ( 2) The single layer of refractory fiber cloth (1) is dried and then laminated under pressure;
    优选地,所述加压的压力为1~10MPa;Preferably, the pressing pressure is 1 to 10 MPa;
    优选地,步骤(2)中,所述加工成型的方法为模切成型。Preferably, in step (2), the method of processing and forming is die cutting.
  9. 根据权利要求5-8任一项所述的制备方法,其中,步骤(2)中,所述耐火纤维布(1)在经过预处理后再与结合剂浆料(2)复合;The preparation method according to any one of claims 5 to 8, wherein in step (2), the refractory fiber cloth (1) is pretreated with a binder slurry (2) after being pretreated;
    优选地,所述预处理为脱浆处理;Preferably, the pretreatment is a desizing treatment;
    优选地,所述脱浆处理的方法包括在乙醇中超声震荡后烘干和/或600℃加热。Preferably, the method for the desizing treatment includes drying and / or heating at 600 ° C. after ultrasonic vibration in ethanol.
  10. 根据权利要求5-9任一项所述的制备方法,其中,所述方法包括以下步骤:The preparation method according to any one of claims 5-9, wherein the method comprises the following steps:
    (1)将配比量的水性聚氨酯、环氧树脂乳液、铝溶胶和分散剂搅拌混合, 得到混合乳液,再向所述混合乳液中加入配比量的填料,经分散后得到所述结合剂浆料(2);(1) Mixing a proportion of a water-based polyurethane, an epoxy resin emulsion, an aluminum sol, and a dispersant to obtain a mixed emulsion, and adding a proportion of a filler to the mixed emulsion to obtain the binder after dispersion. Slurry (2);
    (2)将步骤(1)所得结合剂浆料(2)用涂布或浸渍的方法复合在脱浆处理过的耐火纤维布(1)需要粘合的面上,再对得到的复合了结合剂浆料(2)的耐火纤维布(1)进行叠加,最后模切成型,得到所述密封垫;(2) Combine the binder slurry (2) obtained in step (1) by coating or impregnating method on the surface of the desizing-resistant refractory fiber cloth (1) that needs to be bonded, and then combine the obtained composite Superimposing the refractory fiber cloth (1) of the agent slurry (2), and finally die cutting to obtain the sealing gasket;
    其中,耐火纤维布(1)需要粘合的面上复合的结合剂浆料(2)的量为0.01~0.5g/cm 2,所述叠加的方法为将复合了结合剂浆料(2)的耐火纤维布(1)多层叠加之后再加压烘干或将复合了结合剂浆料(2)的耐火纤维布(1)单层烘干之后再多层加压叠加,所述加压的压力为1~10MPa。 The amount of the binder slurry (2) compounded on the surface to be bonded of the refractory fiber cloth (1) is 0.01 to 0.5 g / cm 2. The superimposing method is to compound the binder slurry (2). Layer of the refractory fiber cloth (1) is laminated and then pressed and dried, or the single layer of the refractory fiber cloth (1) combined with the binder slurry (2) is laminated and laminated and laminated under pressure. The pressure is 1 to 10 MPa.
  11. 如权利要求1-4任一项所述的密封垫的用途,其用于密封刚性异质管件间的连接处。The use of a gasket according to any one of claims 1-4, which is used to seal the connection between rigid heterogeneous pipe fittings.
PCT/CN2018/091743 2018-05-29 2018-06-19 High-temperature resistant, soft and flexible sealing gasket, preparation method thereof, and use thereof WO2019227535A1 (en)

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