CN101195703B - Couplant for fault detection and method for producing the same - Google Patents

Couplant for fault detection and method for producing the same Download PDF

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CN101195703B
CN101195703B CN 200710201516 CN200710201516A CN101195703B CN 101195703 B CN101195703 B CN 101195703B CN 200710201516 CN200710201516 CN 200710201516 CN 200710201516 A CN200710201516 A CN 200710201516A CN 101195703 B CN101195703 B CN 101195703B
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couplant
anti
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CN101195703A (en )
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白敏�
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二重集团(德阳)重型装备股份有限公司
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Abstract

The invention relates to organic chemical technical field, in particular to a soluble anti-corrosion couplant for ultrasonic inspection, and a relative preparation method, wherein the couplant contains 0.5-50% soluble preservative, 10-50% carbowax whose weight average molecular weight M is 400-1000, and 5-50% carbowax whose weight average molecular weight M is 2000-10000, or 10-50% polyether (under 40DEG C, 20000-100000mm<2>/s), 0.01-2% non-silicon compound defoamer, paint, and perfumes, and water of left amount. The couplant has good ultrasonic couple property and good anti-scaling anti-corrosion property on metal, particularly on stainless steel surfacing layer.

Description

一种探伤用耦合剂及其制备方法 One kind of flaw detection coupling agent and preparation method

技术领域 FIELD

[0001] 本发明涉及一种探伤用耦合剂及其制备方法,属于有机化工领域。 [0001] The present invention relates to a flaw detection with a coupling agent and a preparation method, belonging to the field of organic chemicals. 背景技术 Background technique

[0002] 在机械制造、化工等众多行业都需要对工件的焊缝及堆焊层进行无损探伤检测, 比如超声波检测。 [0002] The need to weld overlay and the workpiece in the nondestructive inspection machinery manufacturing, chemical and other industries, such as ultrasonic testing. 当探头和工件表面之间有空气层,超声波的反射率几乎为100%,难以射入工件达不到探伤的目的,因此为了保证超声波的理想传播,实施超声波检测时需要在工件表面涂上一种传递声波的介质即耦合剂。 When the air layer between the probe and the workpiece surface, the ultrasonic reflectance of almost 100%, it is difficult to reach the workpiece incident testing purposes, thus to ensure that the desired propagation of the ultrasonic, ultrasonic testing embodiment involves placing a workpiece surface i.e. species transferred acoustic couplant medium.

[0003] 现有公开的技术资料及中国专利CN1161863A、CN1161863A、CN1070927A等中公开了以水、机油、煤油、甘油、乳化石蜡、羧甲基纤维素、海藻酸钠、丙烯酸聚合物等作为超声波检测耦合剂。 [0003] Information and prior art disclosed in Chinese Patent CN1161863A, CN1161863A, CN1070927A discloses the like with water, oil, kerosene, glycerol, paraffin emulsion, carboxymethyl cellulose, sodium alginate, etc. as an ultrasonic detection acrylic polymer Coupling agent. 这些公开技术虽然能满足人体医用及某些金属超声波检测对耦合剂的要求, 但尚存若干缺陷。 Although these technologies disclosed in the human medical and satisfy certain requirements for ultrasonic testing metal coupling agent, but there are still several drawbacks. 如没有充分考虑耦合剂与金属表面接触后将会引起的变化,没有解决耦合剂中某些成份将造成钢铁表面的堆焊层严重锈蚀,而前述的中国专利CN1161863A的技术领域主要是人体医用超声波检测,CN1161863A、CN1070927A两个中国专利虽然可用于金属超声波检测,但它们的主要目的都是降低成本,并没有把防止钢铁及堆焊层表面的锈蚀作为自己技术发明的重点和关键点;根据金属防腐知识可以了解到在所述的耦合剂中加入三乙醇胺、苯甲酸钠后耦合剂的防锈能力并不强,更不能消除某些离子对不锈钢的晶间腐蚀。 The changes did not fully consider the coupling agent in contact with a metal surface will cause no coupling agent solution will cause some of the ingredients of the steel surface overlay seriously corroded, and the Chinese patent CN1161863A technical field of medical ultrasound main body detecting, CN1161863A, CN1070927A two Chinese Patent Although ultrasonic testing may be used for metal, but their main purpose is to reduce the cost, and does not prevent corrosion of steel and the surface of the overlay and focus their key technologies of the invention; the metal preservative triethanolamine can learn knowledge of the coupling agent, the coupling agent is sodium benzoate anticorrosive ability is not strong, but will not remove some of the ions between the stainless steel corrosion. 同时,根据工件表面粗糙度、耦合剂在工件表面厚度和超声波透射间的关系,在堆焊层表面使用这些耦合剂不能得到理想的耦合效果。 Meanwhile, the surface roughness, the relationship between the coupling agent and the thickness of the surface ultrasonic transmission, using a coupling effect of these coupling agents can not be obtained over the surface of the cladding layer.

[0004] 另外,钢铁的超声波检测还涉及许多重要的其它因素。 [0004] Further, the steel also relate to ultrasonic testing of a number of other factors important. 如当无损探伤是在制造过程结束进行的最终检查,或没有特殊要求时,通常可以使用矿物油一类的材料作为耦合剂, 如牌号为N32的机械油等。 For example, when nondestructive testing during the manufacturing process for the final inspection ends, or there are no special requirements may generally be used a mineral oil-based material as a coupling agent, such as designation of N32 machine oil. 而当制造过程尚未结束,还需对焊缝及堆焊层作消除应力的热处理时,就不能使用矿物油,因为涂施在焊缝及堆焊层表面的矿物油很难完全除去,况且除去的费用十分昂贵,这些残留的矿物油受热后将对焊缝及堆焊层产生危害。 When the manufacturing process is not ended, the need for weld surfacing layer and stress relieving heat treatment time, the mineral oil can not be used, since the surface of the applicator and the weld overlay is difficult to completely remove mineral oil, Moreover removed very expensive to produce, after a mineral oil is heated these residual harmful to weld and weld overlay. 普通矿物油只是在金属表面形成一层油膜,它具有一定的润滑性能,使探伤探头能在焊缝或堆焊层表面自由滑动,但不具备防腐性能,无法防止焊缝及堆焊层在湿热、金属性污染物存在的环境中锈蚀。 Ordinary mineral oil is formed only on the surface layer of the metal film, it has a certain lubricating properties, so that testing probe to slide freely in the weld overlay or surface, but do not have the corrosion resistance can not be prevented in the weld and heat overlay , metal contaminants present in the environment corrosion.

[0005] 为了满足热处理等对耦合剂的要求,在探伤检测中应使用非矿物油型探伤用耦合齐U,目前得到普遍采用的有羧甲基纤维素、聚乙烯醇类、甘油等化学浆糊类物质。 [0005] In order to meet the heat requirements of the coupling agent should be used in non-mineral oil-in flaw detection testing coupled together with U, which is widely used carboxymethylcellulose, polyvinyl alcohol, glycerin and the like chemical pulp paste substances. 如中国专利CN1161863A、CN1038346A、CN1070927A中提出的超声波探伤耦合剂。 Chinese patent CN1161863A, CN1038346A, CN1070927A proposed ultrasonic inspection coupling agent. 这些现有的非矿物油型探伤用耦合剂存在的明显不足是对钢铁的防腐防锈性能较差,探伤检测后的焊缝及堆焊层表面容易出现锈蚀。 These significantly less conventional mineral oil type non-detection of the presence of a coupling agent is poor corrosion preventive properties of the steel, weld overlay and the flaw detection surface prone to corrosion. 而且这些探伤用耦合剂中通常含有使表面致蚀的成分,如氯离子、 醋酸根离子、高浓度的氢氧根离子等,如CN1070927A,CN1161863A均存在这样的的问题;在Cm038346A中还存在使用危害人体健康的亚硝酸盐等问题。 These testing with a coupling agent and usually contain a surface-induced erosion of components, such as chloride, acetate ion, a high concentration of hydroxide ions, such as CN1070927A, CN1161863A there is both a problem; there is also in use in Cm038346A harmful to human health problems such as nitrite. 因此这些探伤用耦合剂特别不适宜于大型化工设备,如加氢反应器及核电反应堆筒体焊缝及堆焊层的超声波探伤。 Thus these testing with a coupling agent particularly unsuitable for large-scale chemical equipment, such as ultrasonic testing hydrogenation reactor and nuclear reactors and tubular body weld surfacing layer. 这类设备的焊缝及堆焊层均是由不锈钢组成,氯离子等卤素对它们的危害作用早已为人们所认识,在选用探伤用耦合剂是必须加以考虑的。 Such equipment and weld surfacing layer are composed of stainless steel, a halogen such as chloride ions harmful effects thereof has long been recognized, the coupling agent is selected flaw detection must be considered. 在生产现场,很容易形成铁素体污染的碳素钢粉尘会对不锈钢产生腐蚀作用,而打磨堆焊不锈钢基体的碳素钢是必须的生产工序,因此要完全消除由此带到焊缝及堆焊层表面的粉尘几乎是不可能的。 In the production site, it is easy to form dust, carbon steel ferritic stainless pollution will have a corrosive effect, while the carbon steel welding polished stainless steel substrate production processes is necessary, whereby so to completely eliminate the weld and brought dust the surface of the cladding layer is almost impossible. 与清除表面使用矿物油的情况相似,凭借清洗的方法清除焊缝及堆焊层表面的粉尘,不仅需要支付颇大的成本,而且还花费很大的工作量,它在实际操作环境中有时是无法清除的。 Using the clear surface similar to mineral oil, and dust remove weld overlay with the surface of the cleaning method, not only need to pay considerable costs, but also takes a lot of work, it is sometimes in the actual operating environment It can not be cleaned. 因此,解决这些腐蚀不仅是保护产品的必然要求而且也是使生产得以顺利进行的重要措施。 Therefore, the solution is not only a necessary requirement for these corrosion protection products but also the production of the smooth conduct of important measures. 其它非矿物油型探伤用耦合剂,如甘油(丙三醇)等,不仅防腐蚀性能与上述矿物油相似,而且它的其它性能如粘度等随温度、水份变化的情况很不理想。 Other non-mineral oil-in testing, such as glycerol (glycerin), not only a corrosion resistance similar to the above-described coupling agent to mineral oil, and its other properties such as viscosity and the like with temperature, the situation is not ideal moisture changes. 温度、水份的微小变化就造成厚度的较大变化,而我们知道厚度与超声波探伤的反射波高密切相关,这种变化给探伤检测带来分析判断上的困难,因而也不适用。 Small changes in temperature, moisture will cause greater changes in thickness, and we know that high is closely related to the thickness of the ultrasonic testing of the reflected wave, this change is difficult to judge on the analysis of flaw detection, and therefore does not apply.

[0006] 综上所述,现有的超声波检测用耦合剂或者不能满足产品制造工艺要求,或者具有性能上的缺陷:如非矿物油型探伤耦合剂防腐性能不佳,在大型化工及核电设备焊缝及堆焊层超声波检测中耦合效果不佳,难以满足工艺及防止不锈钢晶间腐蚀的要求。 [0006] In summary, the conventional ultrasonic testing with a coupling agent or can not meet the requirements of the product manufacturing process, or a defect in performance: non-mineral oil type couplant poor corrosion resistance testing, the large chemical and nuclear power equipment and an ultrasonic weld overlay poor coupling effect is detected, it is difficult to meet the process and prevent the stainless steel intergranular corrosion requirements. 本领域急需开发新的探伤用耦合剂。 An urgent need in the art to develop new testing with a coupling agent.

发明内容 SUMMARY

[0007] 本发明所要解决的技术问题之一是提供一种探伤用耦合剂,该探伤用耦合剂是一种水溶性防锈型超声波探伤用耦合剂,能很好地满足无损探伤检测对超声波耦合及防腐性能的要求,并且容易完全去除。 [0007] One of the present invention to solve the technical problem of providing a testing with a coupling agent, the coupling agent is a detection by ultrasonic testing with a rust-preventive water-soluble coupling agent can satisfy the ultrasonic NDT coupling and corrosion resistance requirements, and easily completely removed.

[0008] 本发明解决该技术问题所采用的技术方案是:本发明探伤用耦合剂,按重量百分比该探伤用耦合剂含有: [0008] Technical Solution The present invention solves this technical problem are: testing with a coupling agent according to the present invention, the percentage by weight comprising testing with a coupling agent:

[0009] 聚乙二醇(重均分子量M = 400〜1000) 10%〜50% [0009] Polyethylene glycol (weight average molecular weight M = 400~1000) 10% ~50%

[0010] 聚乙二醇(重均分子量M = 2000〜10000) 5%〜50% [0010] Polyethylene glycol (weight average molecular weight M = 2000~10000) 5% ~50%

[0011]聚醚(40°C下 20000 〜100000mm2/s) 10%〜50% [0011] Polyether (20000 ~100000mm2 / s at 40 ° C) 10% ~50%

[0012] 水溶性防腐剂 0.5%〜50% [0012] Preservative 0.5% ~ 50% soluble

[0013] 水为余量。 [0013] water balance.

[0014] 进一步地,本发明探伤用耦合剂按重量百分比由以下组分组成: [0014] Further, the present invention is by testing a coupling agent percentage by weight consists of the following components:

[0015] 聚乙二醇(重均分子量M = 400〜1000) 10%〜50% [0015] Polyethylene glycol (weight average molecular weight M = 400~1000) 10% ~50%

[0016] 聚乙二醇(重均分子量M = 2000〜10000) 5 %〜50 % [0016] Polyethylene glycol (weight average molecular weight M = 2000~10000) 5% ~50%

[0017]聚醚(40°C下 20000 〜100000mm2/s) 10%〜50% [0017] Polyether (20000 ~100000mm2 / s at 40 ° C) 10% ~50%

[0018] 水溶性防腐剂 0.5%〜50% [0018] Preservative 0.5% ~ 50% soluble

[0019] 非硅型化合物消泡剂、染料、香料助剂0.01%〜2% [0019] Non-silicon type compound defoamers, dyes, perfumes aid 0.01% ~ 2%

[0020] 水为余量 [0020] water balance

[0021] 本发明所要解决的技术问题另一是提供一种上述探伤用耦合剂的制备方法。 Another [0021] The present invention solves the technical problem is to provide a method for preparing said test couplant.

[0022] 本发明解决该技术问题所采用的技术方案是:本发明的耦合剂的制备方法,包括如下步骤: [0022] Technical Solution The present invention solves this technical problem is: preparation of the present invention the coupling agents, comprising the steps of:

[0023] (1)制备水溶性防腐剂,a.在装有空气冷凝器和温度计的反应装置中,按摩尔比为:脂肪酸0. 85〜1. 05,含氮化合物0. 95〜1. 25,环氧化合物0. 15〜0. 30加入各原料,滴加98%浓硫酸,控制滴加速度,控制体系温度在50°C之内;b.加完后升温至185〜195°C,保温反应1. 5〜2. 5小时,反应生成的水同时被蒸出;C.冷却上述反应物,加入过量的氧化钙,进行蒸馏,馏出液及无水硫酸钠干燥;d.过滤,滤液加入适量活性碳,然后回流30〜50 分钟,收集150〜165°C的馏分制得水溶性防腐剂; [0023] (1) Preparation of a water-soluble preservative, a is in a reaction apparatus fitted with an air condenser and a thermometer, a molar ratio of: 0. 85~1 05 fatty acids, nitrogen-containing compound 0. 95~1. 25, an epoxy compound was added to each 30 0. 15~0 raw materials, 98% concentrated sulfuric acid was added dropwise, the dropping speed control, temperature control system in the 50 ° C;. B addition is complete warm to 185~195 ° C, 1. 5~2 reaction incubated for 5 hours while the water of reaction is distilled off;.. C the reaction was cooled, excess of calcium oxide was distilled, the distillate and dried over anhydrous sodium sulfate;. d filter, the filtrate was added an appropriate amount of activated carbon, and then refluxed for 30 ~ 50 minutes to collect the fraction of 150~165 ° C to obtain a water soluble preservative;

[0024] (2)水溶性防腐剂进一步酯化:在另一反应装置中加入经上述步骤制取的水溶性防腐剂预备物,升温至50士5°C后再加入重均分子量M = 2000〜10000的聚乙二醇并加热至120°C〜140°C,充分搅拌25〜45分钟; [0024] (2) a water soluble preservative further esterified: adding a water soluble preservative composition prepared by the above step of preparation In another reaction apparatus, was heated to 50 [deg.] C before adding persons weight. 5-average molecular weight M = 2000 ~10000 polyethylene glycol and heated to 120 ° C~140 ° C, stir 25~45 minutes;

[0025] (3)加入聚乙二醇(重均分子量M = 400〜1000)和聚醚(40°C下20000〜 100000mm2/s)待产物的粘度达到40°C下50〜150mm2/s之间和酸值小于0. 01时,停止反应; Viscosity [0025] (3) adding polyethylene glycol (weight average molecular weight M = 400~1000) and a polyether (20000~ 100000mm2 / s at 40 ° C) at which the product reaches 40 ° C 50~150mm2 / s of and the acid value is less than 0.01, the reaction was stopped;

[0026] (4)自然冷却,补加余量的蒸馏水,制得水溶性防腐型探伤用耦合剂。 [0026] (4) natural cooling, additional margin of distilled water to obtain a water-soluble anti-corrosion testing with a coupling agent.

[0027] 进一步的技术方案是在上述步骤(4)中,当自然冷却到80°C以下时,还按配制的耦合剂总重量百分比加入0.01%〜2%非硅型化合物消泡剂、染料、香料助剂。 [0027] A further aspect is the above-described step (4), when cooled to below 80 ° C, further weight percent of the total formulation of a coupling agent and 0.01% ~ 2% non-silicone type defoamers compound, dye , perfumery adjuvant.

[0028] 本发明的有益效果是:提供了一种水溶性防锈型超声波探伤用耦合剂,本发明耦合剂为水溶性,它可以用水方便去除,附着在焊缝或堆焊层表面的成分在后续热处理工序中或者自行蒸发、或者不会产生有害产物,本发明耦合剂在探伤过程中及探伤检测之后具有防腐功能,它特别能保护堆焊层表面的蓝色氧化膜不会转变为褐色铁锈。 [0028] Advantageous effects of the invention are: to provide a water-soluble rust ultrasonic testing with a coupling agent, coupling agent of the invention is a water-soluble, it can easily be removed with water, or adhering composition in the weld surfacing layer in a subsequent heat treatment step or self-evaporation, or does not produce harmful products, coupling agent of the present invention prevent corrosion, and after the flaw detection in the detection process, it is particularly to protect the surface of the overlay blue oxide film does not change as a brown rust. 因此,本发明耦合剂对于大型化工和核电设备的焊接质量制造检测具有十分重要的意义。 Thus, the coupling agent of the invention is of great significance for the welding quality and large-scale chemical manufacturing a nuclear detector device. 本发明探伤用耦合剂的制备方法,简单易操作,对制备设备无特殊要求。 The present invention is a testing method for the coupling agent preparation, easy to operate, requires no special preparation equipment.

具体实施方式 detailed description

[0029] 下面结合具体实施方式进一步说明本发明。 [0029] DETAILED DESCRIPTION The following embodiments further illustrate the invention.

[0030] 本发明探伤用耦合剂,按重量百分比含有:水溶性的防腐剂0.5%〜50%、聚乙二醇(重均分子量M = 400〜1000) 10%〜80%和重均分子量M = 2000〜10000的聚乙二醇5%〜50%或聚醚(40°C下20000〜100000mm2/s)10%〜50%等,其中:所述水溶性的防腐剂由C6〜C12脂肪酸、有机胺、环氧化合物在催化剂存在下首先反应而成水溶性防腐剂然后再与聚乙二醇进一步发生反应生成酯; [0030] Inspection of the present invention with a coupling agent, by weight percent comprising: a water-soluble preservative 0.5% ~ 50% polyethylene glycol (weight average molecular weight M = 400~1000) 10% ~80% and the weight average molecular weight M = 2000~10000 polyethylene glycol or polyether 5% ~ 50% (at 40 ° C 20000~100000mm2 / s) 10% ~50% and the like, wherein: the water-soluble preservatives C6~C12 by the fatty acid, organic amine, the epoxy compound is first reacted in the presence of a catalyst formed by a water-soluble preservative and then further reaction with the polyethylene glycol to form an ester;

[0031] 作为一种优选的实施方式,本发明探伤用耦合剂按重量百分比由以下组分组成: 水溶性的防腐剂0. 5%〜50%,聚乙二醇(分子量400〜1000) 10%〜80%和重均分子量M = 2000 〜10000 的聚乙二醇5%〜50%或聚醚(40°C下20000 〜100000mm2/s) 10%〜 50%,非硅型化合物消泡剂、染料、香料助剂0. 01 %〜2%,水为余量。 [0031] As a preferred embodiment, the present invention is by testing a coupling agent percentage by weight consists of the following components: a water-soluble preservative 0.5% ~ 50% polyethylene glycol (molecular weight 400~1000) 10 % ~ 80% and a weight-average molecular weight M = 2000 ~10000 polyethylene glycol or polyether 5% ~ 50% (20000 ~100000mm2 / s at 40 ° C) 10% ~ 50%, non-silicon type defoaming agent compound , dyes, perfumes, 0.01% ~ 2% additives, remainder water.

[0032] 其中,上述水溶性的防腐剂由脂肪酸、含氮化合物、环氧化合物和催化剂在指定条件下反应制备而成,所用各物料的摩尔比为:脂肪酸0. 85〜1. 05、含氮化合物0. 95〜 1. 25、环氧化合物0. 15〜0. 3。 [0032] wherein the water-soluble preservatives nitrogen-containing compound from a fatty acid, prepared by the reaction, an epoxy compound and a catalyst under specified conditions, the materials used in the respective molar ratio: 0. 85~1 05 fatty acid, containing 0. 1.25 95~ nitrogen compound, an epoxy compound 0. 15~0. 3. 所述脂肪酸的碳链为C6〜C18,更具体说它们可以是己酸、 辛酸、癸二酸、月桂酸、油酸中的一种或几种的组合物。 The carbon chain of the fatty acid C6~C18, they may be more specifically caproic acid, caprylic acid, sebacic acid, lauric acid, oleic acid, of one kind or more of a composition. 所述含氮化合物为乙醇胺、二乙醇胺、三乙醇胺、吡啶及其衍生物等,纯度应在99%以上。 The nitrogen-containing compound is ethanolamine, diethanolamine, triethanolamine, pyridine and derivatives thereof, should be more than 99% purity. 所述环氧化合物是环氧乙烷、环氧丙烷,1,4氮氧己烷及其衍生物等催化剂为浓度为98%的硫酸,其用量以控制在体系显酸性为度。 The epoxy compound is a catalyst of ethylene oxide, propylene oxide, 1,4-hexane nitrogen oxides and derivatives thereof to a concentration of 98% sulfuric acid in an amount to control the system as acidic degree.

[0033] 其中,聚醚是由环氧乙烷与环氧丙烷按摩尔比1 : 3的聚合而成,它的粘度为40°C 下20000〜100000mm2/s ;聚乙二醇的重均分子量M = 2000〜10000。 [0033] wherein the polyether is the molar ratio of ethylene oxide and 1 propylene oxide: 3 polymerization, its viscosity at 40 ° C 20000~100000mm2 / s; weight average molecular weight of polyethylene glycol M = 2000~10000. [0034] 上述非硅型化合物消泡剂的作用是减少耦合剂的泡沫,可以采用GXP-112-C、 GXP-112-D等;香料助剂的作用是改善耦合剂气味,可以采用玫瑰香精、芙蓉香精。 [0034] The non-silicon type defoaming agent compound is to reduce the effect of coupling agent foams may be employed GXP-112-C, GXP-112-D and the like; perfumery adjuvant effect is to improve the odor coupling agent, may be employed Rose Perfume , hibiscus flavor. 染料作用是调整耦合剂颜色,可以采用中性玫瑰红染料等。 Dye color effect is to adjust the coupling agent may be neutral rose bengal dye. 这些辅料根据具体需要按本领域的常识进行配合使用。 These materials were blended by using the knowledge in the art according to specific needs.

[0035] 本发明探伤用耦合剂为非矿物油型耦合剂,而且是水溶性的,因此它可以用水方便去除,附着在焊缝或堆焊层表面的成分在后续热处理工序中或者自行蒸发、或者不会产生有害产物,耦合剂在探伤过程中及探伤检测之后具有防腐功能,它特别能保护堆焊层表面的蓝色氧化膜不会转变为褐色铁锈。 [0035] The present invention is by testing the mineral oil is a non-coupling type coupling agent, and is water-soluble, so it can be easily removed with water, adhering to the surface of the component or weld overlay or in a subsequent heat treatment process itself and evaporated or does not produce harmful products, prevent corrosion after couplant and flaw detection testing process, it is particularly blue oxide to protect the surface of the overlay film does not change as a brown rust. 本发明探伤用耦合剂的生产原料来源广泛,均为常见的化工材料,产品及生产成本较低,而且不会对人体及环境产生危害。 The present invention testing with sources of raw materials coupling agent widely, both common chemical materials, products and lower production costs, and will not cause harm to humans and the environment.

[0036] 本发明同时还提供了制备上述探伤用耦合剂的方法,该制备方法简单,对制备设备无特殊要求。 [0036] The present invention also provides a method for preparing said test coupling agent, the preparation method is simple, no special requirements for the preparation of the device. 本发明探伤用耦合剂的制备方法,包括如下步骤:(1)制备水溶性防腐剂, a.在装有空气冷凝器和温度计的反应装置中,按组分加入脂肪酸、环氧化合物和纯度为99%的含氮化合物,滴加98%浓硫酸,控制滴加速度,控制体系温度在50°C之内;b.加完后升温至185〜195°C,保温反应1. 5〜2. 5小时,反应生成的水同时被蒸出;c.冷却上述反应物,加入过量的氧化钙,进行蒸馏,馏出液用无水硫酸钠干燥;d.过滤,滤液加入适量活性碳,然后回流30〜50分钟,收集150〜165°C的馏分制得水溶性防腐剂;(2)在另一反应装置中加入经上述步骤制取的水溶性防腐剂,升温至90士5°C后再加入重均分子量M =2000〜10000的聚乙二醇,充分搅拌,反应25〜45分钟,(3)加入聚乙二醇(分子量M =400〜1000)和聚醚(40°C下20000〜100000mm2/s)待混合物的粘度达到40°C下50〜 150mm2/s和酸值小于0.01时 Flaw detection method for preparing a coupling agent of the present invention, comprising the steps of: (1) Preparation of a water-soluble preservative, a is in a reaction apparatus fitted with an air condenser and a thermometer, was added by a fatty acid component, an epoxy compound and a purity 99% of the nitrogen-containing compound, 98% concentrated sulfuric acid was added dropwise, the dropping speed control, temperature control system in the 50 ° C;. B addition is complete warm to 185~195 ° C, the reaction incubated 5 1. 5~2. hours, while water of reaction is distilled off; C the reaction was cooled, excess of calcium oxide was distilled, the distillate was dried over anhydrous sodium sulfate;. D filtrate appropriate amount of activated carbon was added, then refluxed 30. ~ 50 minutes to collect the fraction of 150~165 ° C to obtain a water soluble preservative; (2) adding water-soluble preservatives prepared by the above steps taken in another reactor, warmed to 90 before adding disabilities 5 ° C M = 2000~10000 weight average molecular weight of polyethylene glycol, stirred well, the reaction 25~45 minutes, (3) addition of polyethylene glycol (molecular weight M = 400~1000) and a polyether (at 40 ° C 20000~100000mm2 / s) viscosity of the mixture to be reached at 40 ° C 50~ 150mm2 / s and an acid value of less than 0.01 停止搅拌;(4)自然冷却,补加余量的蒸馏水,制得水溶性防腐型探伤用耦合剂。 The stirring was stopped; (4) natural cooling, additional margin of distilled water to obtain a water-soluble anti-corrosion testing with a coupling agent. 在所述步骤(4)中,自然冷却到80°C以下时,还可按重量百分比加入0. 01%〜2%非硅型化合物消泡剂、染料、香料助剂。 In the step (4), cooled to below 80 ° C, may also be added in weight percent 0.01% ~ 2% non-silicone antifoaming compounds, dyes, perfumes aid.

[0037] 以下通过具体实施例的方式对本发明做进一步详述,但不应理解为是对本发明主题范围的限定,凡基于上述发明主题作出的修改、替换实现的技术方案均属于本发明的保护范围。 [0037] The following done by way of specific embodiments of the present invention in further detail, but should not be construed as limiting the subject matter the scope of the present invention, all based on the modification described above inventive subject matter made of an alternative implementation of the technical solutions belong to the protection of the present invention. range. 本发明中的mm2/S是指粘度的单位;酸值表示体系中酸性物质的总量,定义为中和Ig树脂所需消耗的氢氧化钾毫克数,以“mg/g”为单位。 The present invention mm2 / S is the unit of viscosity; acid represents the total number of milligrams of potassium hydroxide System acidic substance is defined as a resin and Ig consumption required to "mg / g" units.

[0038] 实施例一制备水溶性防腐剂 [0038] Example Preparation of a water soluble preservative

[0039] (1)、在装有空气冷凝器和温度计的反应装置中,按组分加入月桂酸1摩尔,含氮化合物吡啶1. 15摩尔,环氧丙烷0. 2摩尔,滴加98%浓硫酸,控制滴加速度使反应体系为酸性,控制体系温度在50°C之内; [0039] (1), in a reaction apparatus fitted with an air condenser and a thermometer, 1 mol of lauric acid is added according to the components, nitrogen-containing compound pyridine 1.15 moles, 0.2 moles of propylene oxide was added dropwise 98% concentrated sulfuric acid, the control of dropping the reaction system acidic, the temperature control system in the 50 ° C;

[0040] (2)、加完后升温至185〜195°C,保温反应1. 5〜2. 5小时,反应生成的水同时被蒸出;c.冷却上述反应物,加入过量的氧化钙,进行蒸馏,馏出液用无水硫酸钠干燥; [0040] (2). After the addition was heated to 185~195 ° C, the reaction incubated 1. 5~2 5 hours, while water of reaction is distilled off;. C The reaction was cooled, excess of calcium oxide. , distillation, distillate dried over anhydrous sodium sulfate;

[0041] (3)、过滤,滤液加入适量活性碳,然后回流30〜50分钟,收集150〜165°C的馏分,制得水溶性防腐剂。 [0041] (3), filtered, and the filtrate was added an appropriate amount of activated carbon, and then refluxed for 30 ~ 50 minutes to collect the fraction of 150~165 ° C, to obtain a water-soluble preservative.

[0042] 重复上述步骤,制备所需量的水溶性防腐剂。 [0042] The above steps are repeated, to produce the desired amount of water-soluble preservatives.

[0043] 实施例二制备本发明探伤用耦合剂 [0043] The two embodiments of the present invention was prepared using a coupling agent embodiment testing

[0044] (1)在2000ml三颈瓶中加入实施例一制备的水溶性防腐剂100克,升温至90士5°C后再加分子量6000的聚乙二醇300克,充分搅拌25分钟后,待反应物的酸值<0.01mg/g,粘度达到1650mm2/S以上后,加入聚乙二醇(分子量M = 400) 500克和粘度为40°C下25000mm2/S的聚醚250克加热至温度控制在40°C〜45°C,待产物的粘度达到60〜 70mm2/s(40°CT )之间,酸值小于0. 01时,停止反应; After [0044] (1) in 2000ml three-necked flask was added a water soluble preservative prepared according to Example 100 grams, was heated to 90 [deg.] C together with disabilities molecular weight. 5 glycol 6000 300 g, sufficiently stirred for 25 minutes after an acid value of <0.01mg / g to be reactants, the viscosity is 1650mm2 / S or more, the addition of polyethylene glycol (molecular weight M = 400) 500 g of a polyether and a viscosity at 40 ° C 25000mm2 / S 250 gram of hot to a temperature controlled at 40 ° C~45 ° C, the viscosity of the product to be reached between 60~ 70mm2 / s (40 ° CT), the acid value is less than 0.01, the reaction was stopped;

[0045] (2)停止反应后自然冷却到80°C以下,充分搅拌后补加余量的蒸馏水340克,再搅拌3〜5分钟即可。 After natural cooling [0045] (2) to stop the reaction below 80 ° C, supplemented with a balance of 340 g of distilled water was sufficiently stirred, and then stirred for 3 to 5 minutes. 这样就得到本发明所述的探伤用防腐型耦合剂。 Thus obtained preservative detection type coupling agents according to the present invention.

[0046] 实施例三制备本发明探伤用耦合剂 [0046] Inspection with a coupling agent was prepared according to a third embodiment of the present invention

[0047] (1)在3000ml三颈瓶中加入实施例一制备的水溶性防腐剂200克,升温至90士5 °C后再加的分子量8000聚乙二醇100克,充分搅拌30分钟,待反应物的酸值 [0047] (1) in 3000ml three-necked flask was added a water soluble preservative prepared according to Example 200 g, was heated to 90 [deg.] C together with disabilities molecular weight. 5, polyethylene glycol 8000 100 g, sufficiently stirred for 30 minutes, the acid value of the reactants to be

< 0.01mg/g,粘度> 1650mm2/S后,加入聚乙二醇(分子量M = 800) 790克,粘度为40°C下45000mm2/s的聚醚350克、加热至45°C〜50°C,待产物的粘度达到60〜70mm7s(40°C下) 之间,酸值小于0.01时,停止反应; <0.01mg / g, viscosity> 1650mm2 / S, a solution of polyethylene glycol (molecular weight M = 800) 790 g, a viscosity at 40 ° C for 45000mm2 / s polyethers 350 g, was heated to 45 ° C~50 ° C viscosity, the product to be reached between 60~70mm7s (at 40 ° C), the acid value is less than 0.01, the reaction was stopped;

[0048] (2)停止反应后自然冷却到80°C以下,等比加入助剂非硅型化合物消泡剂GXP-112-D、中性玫瑰红染料、芙蓉香精共10克(0. 6% ),充分搅拌后补加余量的蒸馏水150 克,再搅拌3〜5分钟即可。 [0048] (2) is stopped to cool to below 80 ° C After the reaction, adding additives geometric non-silicon type defoaming agent compound GXP-112-D, neutral red dye rose, hibiscus flavor total of 10 g (0.6 %), thoroughly stirred additional balance 150 g of distilled water, and then stirred for 3 to 5 minutes.

[0049] 实施例四制备本发明探伤用耦合剂 [0049] Inspection with a coupling agent according to a fourth embodiment of the present invention was prepared

[0050] (1)在500ml三颈瓶中加入实施例一制备的水溶性防腐剂90克,升温至90士5°C 后再加分子量10000的聚乙二醇235克,充分搅拌40分钟,待反应物的酸值< 0. 01mg/g,粘度彡1650mm2/s后,加入聚乙二醇(分子量M= 1000) 50克,粘度为40°C下65000mm2/s聚醚10克加热至温度控制在40°C〜45°C,待产物的粘度达到60〜70mm7S(40°C下)之间, 酸值小于0.01时,停止反应; [0050] (1) In a three-necked 500ml flask was added an aqueous preservative prepared according to Example 90 g, heated to 90 [deg.] C together with disabilities MW 10,000. 5 polyethylene glycol 235 g, sufficiently stirred for 40 minutes, the acid value of the reaction product to be <0. 01mg / g, the viscosity of San 1650mm2 / s, the addition of polyethylene glycol (molecular weight M = 1000) 50 g and viscosity at 40 ° C for 65000mm2 / s 10 g of the polyether heated to a temperature control 40 ° C~45 ° C, the viscosity of the product to be reached between the (at 40 ° C) 60~70mm7S, the acid value is less than 0.01, the reaction was stopped;

[0051] (2)停止反应后自然冷却到80°C以下,加入助剂非硅型化合物消泡剂GXP-112-D、 中性玫瑰红染料、芙蓉香精共1克,充分搅拌后补加余量的蒸馏水19克,再搅拌3〜5分钟即可。 [0051] (2) The reaction was stopped to cool to below 80 ° C, non-silicon type compound added to aid defoamer GXP-112-D, neutral red dye rose, hibiscus essence of 1 g. After stirring additional 19 g distilled water balance, and then stirred for 3 to 5 minutes.

[0052] 实施例五制备本发明探伤用耦合剂 [0052] Inspection with a coupling agent according to a fifth embodiment of the present invention was prepared

[0053] (1)在10升反应釜中加入实施例一制备的水溶性防腐剂1.5公斤,升温至90士5°C后再加分子量6000的聚乙二醇1.8公斤,充分搅拌35分钟,待反应物的酸值 After [0053] (1) addition of a water soluble preservative prepared according to Example 10 1.5 kg liter reaction kettle was warmed to 90 [deg.] C together with disabilities molecular weight polyethylene. 5 glycol 6000 1.8 kg, sufficiently stirred for 35 minutes, the acid value of the reactants to be

< 0.01mg/g,粘度> 1650mm2/s后,加入聚乙二醇(分子量M = 600) 2. 5公斤,40°C下45000mm2/s的聚醚0. 2公斤加热至45°C〜50°C,待产物的粘度达到60〜70mm2/s (40°C下) 之间,酸值小于0.01时,停止反应; After <0.01mg / g, viscosity> 1650mm2 / s, the addition of polyethylene glycol (molecular weight M = 600) 2. 5 kilograms, 40 ° C under 45000mm2 / s 0.2 kg of the polyether was heated to 45 ° C~50 ° C, the viscosity of the product to be reached between the (at 40 ° C) 60~70mm2 / s, the acid value is less than 0.01, the reaction was stopped;

[0054] (2)停止反应后自然冷却到80°C以下,加入助剂非硅型化合物消泡剂GXP-112-C、 中性玫瑰红染料、玫瑰香精共0. 02公斤,充分搅拌后补加余量的蒸馏水1. 48公斤,再搅拌3〜5分钟即可。 After [0054] (2) After the reaction was stopped to cool to below 80 ° C, non-silicon type compound added to aid defoamer GXP-112-C, rose neutral red dye, a total of 0.02 kg rose essence, stir the balance of distilled water supplemented with 1.48 kg, stirred for 3 to 5 minutes.

[0055] 试验例一本发明耦合剂的性能检测试验 [0055] Performance Testing Test Example of the present invention a coupling agent

[0056] 上述各实施例二到五所制得耦合剂的性能检测结果如下: [0056] The performance test result of each example two to five coupling agent is prepared as follows:

[0057] 1耦合性能:用友联PXUT-360超声波探伤仪在厚度为200mm、不锈钢堆焊层厚度为70mm钢件上进行几种耦合剂的对比检测其结果是: [0057] The coupler performance: PXUT-360 by Union ultrasonic flaw detector having a thickness of 200mm, stainless steel weld a layer thickness of several comparison couplant on a detection result thereof is 70mm steel:

[0058] 耦合剂名称;机油甘油工业浆糊本发明各实施例结果平均值 [0058] The coupling agent name; average results of each example embodiment of the present invention is a paste of oil industry glycerol

[0059]波高(Db) 10 20 15 36 [0059] The wave height (Db) 10 20 15 36

[0060] 同时,本发明各实施例制备的耦合剂的其它声学性能检测结果平均值是:声速(M/s) : 1980;声阻抗(X106g/cm. s) : 1.97,超声衰减(dB/cm. Μ) :^ 0. 03[0061] 2本发明耦合剂的防锈防腐蚀性能如表1所示: Other acoustic properties of the detection result of the average [0060] Meanwhile, various embodiments of the present invention is prepared according to the coupling agent is: sound velocity (M / s): 1980; acoustic impedance (X106g / cm s.): 1.97, ultrasonic attenuation (dB / . cm Μ): ^ 0. 03 [0061] 2 rust and corrosion the present invention is capable of coupling agent shown in table 1:

[0062] 表一本发明耦台剂性能检测结果 [0062] TABLE invention is a coupling agent station performance testing results

[0063] [0063]

Figure CN101195703BD00101

[0064] 因此,从上述声学性能、在不锈钢表面与超声波的耦合性能及防锈防腐蚀性能等实测数据我们可以看出本发明的耦合剂与已有的耦合剂相比,不光具有优良的耦合性能, 而且还具有其它耦合剂完全不具备的防锈防腐及工艺优点。 [0064] Thus, from the above-described acoustic performance, the performance of the stainless steel surface in the coupling of the ultrasonic energy and the like rust and corrosion experimental data we can see that the coupling agent of the invention as compared with conventional coupling agents not only have excellent coupling performance, but also has the advantages of rust and corrosion and other processes do not have any of the coupling agents. 此外,本发明的探伤用耦合剂的生产原料成本低,毒性小,同时本发明的探伤用耦合剂的制备方法简单,对制备设备无特殊要求,得到的探伤用耦合剂对人体安全可靠,为大型化工及核电设备焊缝及堆焊层探伤检查提供了一种新的性能优良的必需材料,具有很好的应用前景。 Preparation Further, the low raw material cost of testing with a coupling agent of the present invention, low toxicity, while the present invention flaw detection couplant simple, no special requirements for the preparation of the device, obtained testing with a coupling agent for human safety and reliability, as large chemical and nuclear power equipment and weld overlay inspection techniques provide a new excellent properties necessary material having good prospects.

Claims (14)

  1. 1. 一种探伤用耦合剂,其特征在于:按重量百分比该探伤用耦合剂含有:重均分子量M=400〜1000的聚乙二醇 10%〜50%重均分子量M=2000〜10000的聚乙二醇 5%〜50%40°C下粘度为20000〜100000 mm2/s的聚醚10%〜50% 水溶性防腐剂 0. 5%〜50%水为余量;所述水溶性防腐剂由脂肪酸、含氮化合物和环氧化合物三种成分经酸催化反应制备而成;所用三种成分的摩尔比为:脂肪酸0.85〜1.05、含氮化合物0. 95〜1. 25、环氧化合物0. 15 〜0. 3。 A testing with a coupling agent, wherein: the percentage by weight of the coupling with a detection agent comprising: M = 400~1000 weight average molecular weight polyethylene glycol 10% ~ 50%, weight average molecular weight of M = 2000~10000 the polyethylene glycol 5% ~50% 40 ° C viscosity 20000~100000 mm2 / s 10% ~ 50% of a water-soluble polyether preservative 0.5% ~ 50% balance water; the water soluble preservative agent from fatty acids, nitrogen-containing compound and an epoxy compound prepared by three components obtained by acid-catalyzed reactions; molar ratio of the three components is used: 0.85~1.05 fatty acids, nitrogen-containing compound 0. 95~1 25, an epoxy compound. 0.15 ~ 0. 3. 所述探伤用耦合剂通过如下步骤制得:(1)制备水溶性的防腐剂:a.在装有空气冷凝器和温度计的反应装置中,按摩尔比为0.85〜1.05 : 0.95〜1.25 : 0. 15〜0. 3分别加入脂肪酸、含氮化合物和环氧化合物,滴加98%浓硫酸,控制滴加速度,以保证体系温度控制在50°C之内;b.加完后升温至185〜195°C,保温反应1. 5〜2. 5小时,反应生成的水同时被蒸出;c.冷却上述反应物,加入硫酸摩尔数2倍量的氧化钙,进行蒸馏,馏出液及无水硫酸钠干燥;d.过滤,滤液中加入1/8体积的活性碳,然后回流30〜50分钟,收集150〜 165°C的馏分制得水溶性防腐剂;(2)在另一反应装置中加入经上述步骤制取的水溶性防腐剂,升温至50士5°C后加入重均分子量M = 2000〜10000的聚乙二醇,加热至120°C〜140°C,充分搅拌25〜45分钟;(3)再加入分子量M = 400〜1000的聚乙二醇和聚醚,待产物的粘度达 The testing with a coupling agent prepared by the following steps: (1) Preparation of water-soluble preservatives:. A reaction apparatus equipped with an air condenser and a thermometer, a molar ratio of 0.85~1.05: 0.95~1.25: 0 . 15~0 3 fatty acids were added, the nitrogen-containing compound and an epoxy compound, 98% concentrated sulfuric acid was added dropwise, dropping control to ensure that the temperature of the system is controlled within 50 ° C of; B addition is complete warm to 185~. 195 ° C, the reaction incubated 1. 5~2 5 hours, while water of reaction is distilled off;.. c the reaction was cooled, added to 2 times the amount of calcium oxide moles of sulfuric acid, it is distilled, and the distillate no over anhydrous sodium sulfate; D filtration, the filtrate was added 1/8 volume of activated carbon, and then refluxed for 30 ~ 50 minutes to collect the fraction of manufactured 150~ 165 ° C to obtain a water soluble preservative;. (2) in another reaction apparatus water soluble preservatives were added after the preparation of the above-described steps, the added weight was warmed to 50 [deg.] C-average molecular weight disabilities. 5 M = 2000~10000 polyethylene glycol, heated to 120 ° C~140 ° C, stir 25~ 45 minutes; (3) a molecular weight M = 400~1000 added polyethylene glycol and a polyether, the viscosity of the product to be 40°C下50〜 150mm2/s之间和酸值小于0. 01时,停止反应;(4)自然冷却,补加余量的蒸馏水,制得水溶性防腐型探伤用耦合剂。 At 40 ° C 50~ 150mm2 / s between 0.5 and acid number below 01, the reaction was stopped; (4) natural cooling, additional margin of distilled water to obtain a water-soluble anti-corrosion testing with a coupling agent.
  2. 2.根据权利要求1所述探伤用耦合剂,其特征在于:所述脂肪酸的碳链为C6〜C18,为己酸、辛酸、癸二酸、月桂酸、油酸中的至少一种。 2. The flaw detection according to claim 1 with a coupling agent, characterized in that: the fatty acid carbon chain of C6~C18, as caproic acid, caprylic acid, sebacic acid, lauric acid, at least one of oleic acid.
  3. 3.根据权利要求1所述探伤用耦合剂,其特征在于:所述含氮化合物为乙醇胺、二乙醇胺、三乙醇胺或吡啶中的至少一种。 1 according to the testing with a coupling agent as claimed in claim, wherein: the nitrogen-containing compound is ethanolamine, diethanolamine, triethanolamine or at least one of pyridine.
  4. 4.根据权利要求1所述探伤用耦合剂,其特征在于:所述环氧化合物是环氧乙烷或环氧丙烷中的至少一种。 4. The flaw detection according to claim 1 with a coupling agent, wherein: said epoxy compound is at least one of ethylene oxide or propylene oxide.
  5. 5.根据权利要求1所述探伤用耦合剂,其特征在于:所述催化反应过程中,催化剂为浓度98%的硫酸,其用量以控制到体系显酸性为准。 1 according to the testing with a coupling agent as claimed in claim, wherein: the catalytic reaction process, the concentration of catalyst is 98% sulfuric acid in an amount to control the system to acidic prevail.
  6. 6.根据权利要求1所述探伤用耦合剂,其特征在于:所述聚醚是由环氧乙烷与环氧丙烷按摩尔比1 : 3聚合而成,它的粘度为40°C下20000〜100000mm2/s。 According to claim 1 testing with a coupling agent, wherein: said molar ratio of 1 polyethers are ethylene oxide and propylene oxide: 3 polymerization, its viscosity at 40 ° C 20000 ~100000mm2 / s.
  7. 7.制备权利要求1所述探伤用耦合剂的方法,包括如下步骤:(1)制备水溶性的防腐剂:a.在装有空气冷凝器和温度计的反应装置中,按摩尔比为0. 85〜1. 05 : 0. 95〜1. 25 : 0. 15〜0. 3分别加入脂肪酸、含氮化合物和环氧化合物,滴加98%浓硫酸,控制滴加速度,以保证体系温度控制在50°C之内;b.加完后升温至185〜 195°C,保温反应1. 5〜2. 5小时,反应生成的水同时被蒸出;c.冷却上述反应物,加入硫酸摩尔数2倍量的氧化钙,进行蒸馏,馏出液及无水硫酸钠干燥;d.过滤,滤液中加入1/8体积的活性碳,然后回流30〜50分钟,收集150〜165°C的馏分制得水溶性防腐剂;(2)在另一反应装置中加入经上述步骤制取的水溶性防腐剂,升温至50士5°C后加入重均分子量M = 2000〜10000的聚乙二醇,加热至120°C〜140°C,充分搅拌25〜45分钟;(3)再加入分子量M = 400〜1000的聚乙二醇和聚 7. The flaw detection method for the coupling agent preparation as claimed in claim 1, comprising the steps of: (1) Preparation of water-soluble preservatives:. A In a reaction device equipped with an air condenser and a thermometer, a molar ratio of 0. 85~1 05: 0. 95~1. 25: 0. 15~0 3 fatty acids were added, the nitrogen-containing compound and an epoxy compound, 98% concentrated sulfuric acid was added dropwise, the dropping speed control, temperature control system to ensure of the 50 ° C;. B addition is complete warm to 185~ 195 ° C, the reaction incubated 1. 5~2 5 hours, while water of reaction is distilled off;. C the reaction was cooled, added to the number of moles of sulfuric acid. 2 times the amount of calcium oxide was distilled, and the distillate was dried over anhydrous sodium sulfate;. d was filtered, the filtrate was added 1/8 volume of activated carbon, and then refluxed for 30 ~ 50 minutes to collect the fraction 150~165 ° C obtain a water soluble preservative; (2) adding water-soluble preservatives prepared by the above steps taken in another reactor, warmed to 50 [deg.] C was added Disabled weight average. 5 M = 2000~10000 molecular weight polyethylene glycol and heated to 120 ° C~140 ° C, stir 25~45 min; (3) M = molecular weight of the added polyethylene glycol and polyethylene 400~1000 醚,待产物的粘度达到40°C下50〜 150mm2/s之间和酸值小于0. 01时,停止反应;(4)自然冷却,补加余量的蒸馏水,制得水溶性防腐型探伤用耦合剂。 Ethers, the viscosity of the product to be reached at between 40 ° C 50~ 150mm2 / s and an acid value of less than 0. 01, the reaction was stopped; (4) natural cooling, additional margin of distilled water to obtain a water-soluble anti-corrosion testing with a coupling agent.
  8. 8. 一种探伤用耦合剂,其特征在于:按重量百分比该探伤用耦合剂由以下组分组成:重均分子量M=400〜1000的聚乙二醇 10%〜50%;重均分子量M=2000〜10000的聚乙二醇 5%〜50%;40°C下粘度为20000〜100000 mm2/s的聚醚10%〜50%;水溶性防腐剂 0. 5%〜50%;助剂 0. 01%〜2%;水为余量;其中助剂为非硅型消泡剂、染料或香料中的至少一种;所述水溶性防腐剂由脂肪酸、含氮化合物和环氧化合物三种成分经酸催化反应制备而成;所用三种成分的摩尔比为:脂肪酸0.85〜1.05、含氮化合物0. 95〜1. 25、环氧化合物0. 15 〜0. 3 ;所述探伤用耦合剂通过如下步骤制得:(1)制备水溶性的防腐剂:a.在装有空气冷凝器和温度计的反应装置中,按摩尔比为0.85〜1.05 : 0.95〜1.25 : 0. 15〜0. 3分别加入脂肪酸、含氮化合物和环氧化合物,滴加98%浓硫酸,控制滴加速度,以保证体系温度控制在50°C之内; A testing with a coupling agent, wherein: percentage by weight of the coupling agent with the detection comprises the following components: M = 400~1000 weight average molecular weight polyethylene glycol 10% ~ 50%; weight average molecular weight M = 2000~10000 polyethylene glycol 5% ~ 50%; 40 ° C for viscosity 20000~100000 mm2 / s 10% ~ 50% of the polyether; aqueous preservative 0.5% ~ 50%; aid 0.01% ~ 2%; the balance water; wherein the at least one auxiliary non-silicone type defoamers, dyes or perfumes; preservatives from fatty acids of the water-soluble, nitrogen-containing compound and an epoxy compound three ingredients prepared by acid catalyzed reaction formed; molar ratio of the three components is used: 0.85~1.05 fatty acids, nitrogen-containing compound 95~1 0. 25, 0.15 ~ 0 3 epoxy compound; with the testing. couplant prepared by the following steps: (1) preparation of water-soluble preservatives:. a reaction apparatus fitted with an air condenser and a thermometer, a molar ratio of 0.85~1.05: 0.95~1.25: 0. 15~0 3 fatty acids were added, the nitrogen-containing compound and an epoxy compound, 98% concentrated sulfuric acid was added dropwise, dropping control to ensure that the temperature of the system is controlled within the 50 ° C; b.加完后升温至185〜195°C,保温反应1. 5〜2. 5小时,反应生成的水同时被蒸出;c.冷却上述反应物,加入硫酸摩尔数2倍量的氧化钙,进行蒸馏,馏出液及无水硫酸钠干燥;d.过滤,滤液中加入1/8体积的活性碳,然后回流30〜50分钟,收集150〜 165°C的馏分制得水溶性防腐剂;(2)在另一反应装置中加入经上述步骤制取的水溶性防腐剂,升温至50士5°C后加入重均分子量M = 2000〜10000的聚乙二醇,加热至120°C〜140°C,充分搅拌25〜45分钟;(3)再加入分子量M = 400〜1000的聚乙二醇和聚醚,待产物的粘度达到40°C下50〜 150mm2/s之间和酸值小于0. 01时,停止反应;(4)自然冷却,补加余量的蒸馏水,制得水溶性防腐型探伤用耦合剂;所述步骤⑷中,自然冷却到80°C以下时,还按重量百分比加入0.01%〜2%助剂,所述助剂为非硅型消泡剂、染料或香料中的至少一种。 . B After the addition was heated to 185~195 ° C, the reaction incubated 1. 5~2 5 hours, while water of reaction is distilled off;.. C The reaction was cooled, added to 2 times the amount of calcium oxide moles of sulfuric acid , distillation, distillate and dried over anhydrous sodium sulfate;. d was filtered, the filtrate was added 1/8 volume of activated carbon, and then refluxed for 30 ~ 50 minutes to collect the fraction 150~ 165 ° C to obtain a water soluble preservative ; (2) Preparation by the above step was added in a further reaction apparatus aqueous preservative, was heated to 50 [deg.] C was added Disabled weight average. 5 M = 2000~10000 molecular weight polyethylene glycol, heated to 120 ° C ~140 ° C, stir 25~45 min; (3) a molecular weight M = 400~1000 added polyethylene glycol and polyethers, reached between the viscosity of the product to be 40 ° C 50~ 150mm2 / s and an acid when less than 0. 01, the reaction was stopped; (4) natural cooling, additional margin of distilled water to obtain a water-soluble anti-corrosion testing with a coupling agent; ⑷ in said step, cooled to below 80 ° C, further press by weight and 0.01% ~ 2% adjuvant, said adjuvant least one non-silicon type defoaming agents, dyes or perfumes.
  9. 9.根据权利要求8所述探伤用耦合剂,其特征在于:所述脂肪酸的碳链为C6〜C18,为己酸、辛酸、癸二酸、月桂酸、油酸中的至少一种。 9. The flaw detection according to claim 8 with a coupling agent, characterized in that: the fatty acid carbon chain of C6~C18, as caproic acid, caprylic acid, sebacic acid, lauric acid, at least one of oleic acid.
  10. 10.根据权利要求8所述探伤用耦合剂,其特征在于:所述含氮化合物为乙醇胺、二乙醇胺、三乙醇胺或吡啶中的至少一种。 10. The flaw detection according to claim 8 with a coupling agent, wherein: the nitrogen-containing compound is ethanolamine, diethanolamine, triethanolamine or at least one pyridine.
  11. 11.根据权利要求8所述探伤用耦合剂,其特征在于:所述环氧化合物是环氧乙烷或环氧丙烷中的至少一种。 11. The flaw detection according to claim 8 with a coupling agent, wherein: said epoxy compound is at least one of ethylene oxide or propylene oxide.
  12. 12.根据权利要求8所述探伤用耦合剂,其特征在于:所述催化反应过程中,催化剂为浓度98%的硫酸,其用量以控制到体系显酸性为准。 12. The flaw detection according to claim 8 with a coupling agent, wherein: the catalytic reaction process, the concentration of catalyst is 98% sulfuric acid in an amount to control the system to acidic prevail.
  13. 13.根据权利要求8所述探伤用耦合剂,其特征在于:所述聚醚是由环氧乙烷与环氧丙烷按摩尔比1 : 3聚合而成,它的粘度为40°C下20000〜100000mm2/s。 Under polymerization 200,003, its viscosity is 40 ° C: 13. flaw detection according to claim 8 with a coupling agent, wherein: said molar ratio of 1 polyethers are ethylene oxide and propylene oxide ~100000mm2 / s.
  14. 14.制备权利要求8所述探伤用耦合剂的方法,包括如下步骤:(1)制备水溶性的防腐剂:a.在装有空气冷凝器和温度计的反应装置中,按摩尔比为0. 85〜1. 05 : 0. 95〜1. 25 : 0. 15〜0. 3分别加入脂肪酸、含氮化合物和环氧化合物,滴加98%浓硫酸,控制滴加速度,以保证体系温度控制在50°C之内;b.加完后升温至185〜 195°C,保温反应1. 5〜2. 5小时,反应生成的水同时被蒸出;c.冷却上述反应物,加入硫酸摩尔数2倍量的氧化钙,进行蒸馏,馏出液及无水硫酸钠干燥;d.过滤,滤液中加入1/8体积的活性碳,然后回流30〜50分钟,收集150〜165°C的馏分制得水溶性防腐剂;(2)在另一反应装置中加入经上述步骤制取的水溶性防腐剂,升温至50士5°C后加入重均分子量M = 2000〜10000的聚乙二醇,加热至120°C〜140°C,充分搅拌25〜45分钟;(3)再加入分子量M = 400〜1000的聚乙二醇和 14. A method of testing with a coupling agent in the preparation as claimed in claim 8, comprising the steps of: (1) Preparation of water-soluble preservatives:. A In a reaction device equipped with an air condenser and a thermometer, a molar ratio of 0. 85~1 05: 0. 95~1. 25: 0. 15~0 3 fatty acids were added, the nitrogen-containing compound and an epoxy compound, 98% concentrated sulfuric acid was added dropwise, the dropping speed control, temperature control system to ensure of the 50 ° C;. B addition is complete warm to 185~ 195 ° C, the reaction incubated 1. 5~2 5 hours, while water of reaction is distilled off;. C the reaction was cooled, added to the number of moles of sulfuric acid. 2 times the amount of calcium oxide was distilled, and the distillate was dried over anhydrous sodium sulfate;. d was filtered, the filtrate was added 1/8 volume of activated carbon, and then refluxed for 30 ~ 50 minutes to collect the fraction 150~165 ° C obtain a water soluble preservative; (2) adding water-soluble preservatives prepared by the above steps taken in another reactor, warmed to 50 [deg.] C was added Disabled weight average. 5 M = 2000~10000 molecular weight polyethylene glycol and heated to 120 ° C~140 ° C, stir 25~45 min; (3) a molecular weight M = 400~1000 added polyethylene glycol and 醚,待产物的粘度达到40°C下50〜 150mm2/s之间和酸值小于0. 01时,停止反应;(4)自然冷却,补加余量的蒸馏水,制得水溶性防腐型探伤用耦合剂;所述步骤⑷中,自然冷却到80°C以下时,还按重量百分比加入0.01%〜2%助剂,所述助剂为非硅型消泡剂、染料或香料中的至少一种。 Ethers, the viscosity of the product to be reached at between 40 ° C 50~ 150mm2 / s and an acid value of less than 0. 01, the reaction was stopped; (4) natural cooling, additional margin of distilled water to obtain a water-soluble anti-corrosion testing with a coupling agent; ⑷ in said step, cooled to below 80 ° C, further weight percent solution of 0.01% ~ 2% adjuvant, the non-silicon defoamer additives, dyes or perfumes least one kind.
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