CN102127197A - Preparation method for phenolic resin for magnesia-carbon brick - Google Patents

Preparation method for phenolic resin for magnesia-carbon brick Download PDF

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CN102127197A
CN102127197A CN 201010568441 CN201010568441A CN102127197A CN 102127197 A CN102127197 A CN 102127197A CN 201010568441 CN201010568441 CN 201010568441 CN 201010568441 A CN201010568441 A CN 201010568441A CN 102127197 A CN102127197 A CN 102127197A
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magnesia
phenolic resin
phenol
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carbon brick
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CN102127197B (en )
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唐路林
胡伟
魏务翠
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山东圣泉化工股份有限公司
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Abstract

The invention discloses a preparation method of phenolic resin for a magnesia-carbon brick. The method comprises the following steps of: (1) adding phenol, formaldehyde and an alkaline catalyst into a reaction kettle in the mass ratio of 1.0:(1.1-1.5):(0.01-0.03), raising the temperature to 60-90 DEG C and preserving heat for 1-4 hours; (2) adding papermaking waste liquor and alcohol substances into the reaction kettle and stirring uniformly, wherein the weight of the papermaking waste liquor is 10-20 percent of that of phenol, and the weight of the alcohol substances is 2-5 percent of that of the phenol; and (3) performing vacuum distillation on a uniform mixture obtained in the step (2) at the temperature between 60 DEG C and 90 DEG C until the viscosity of the uniform mixture is between 3,000 MPa.s per 25 DEG C and 25,0000 MPa.s per 25 DEG C. The magnesia-carbon brick obtained by mixing the phenolic resin prepared with the method with magnesia aggregate, magnesia fine powder and graphite and molding has high mechanical property, high compressive strength and high high-temperature breaking strength; meanwhile, the phenolic resin has low preparation cost, so that the production cost of the magnesia carbon brick is greatly lowered.

Description

镁碳砖用酚醛树脂的制备方法 Preparation of phenolic resin MgO-C

技术领域 FIELD

[0001] 本发明涉及酚醛树脂技术领域,尤其是用作镁碳耐火砖结合剂的酚醛树脂的制备方法。 [0001] Technical Field The present invention relates to a phenolic resin, particularly MgO-C bricks prepared as phenolic resin binder.

背景技术 Background technique

[0002] 镁碳耐火材料,是以氧化镁和碳为主要成分的耐火材料。 [0002] MgO-C refractories, and magnesia based refractory material mainly composed of carbon. 具有优良的抗渣侵蚀性、 熔渣渗透性、热震稳定性和导热性。 Has excellent slag resistance, the slag penetration, thermal shock resistance and thermal conductivity. 显气孔率为3%〜10%。 Apparent porosity of 3% ~ 10%. 主要用于炼钢氧化转炉的炉衬、出钢口,高功率电炉炉墙热点部位,以及炉外精炼炉内衬、盛钢桶渣线部位等。 Oxidation mainly for lining steel converter, tapping hole, high power electric furnace wall hot spots, and the refining furnace lining furnace, ladle slag line and the like. 一般采用高纯镁砂粉粒、碳素材料(包括石墨)和焦油浙青或树脂等为原料,经配料、热混、成型后, 再经300°C左右或1000°C以上焙烧而成。 Usually high-purity magnesia particles, carbon material (including graphite), and cyan, or tar Zhejiang resin as raw materials, ingredients, hot mix, forming, and then roasting was about 300 ° C or above 1000 ° C.

[0003] 镁碳耐火材料的应用历史悠长,应用范围广泛,尤其是镁碳砖,已经在转炉、电炉、 钢包以及炉外精炼等方面得到了很好的应用。 [0003] Application of a long history of MgO-C refractories, wide range of applications, particularly MgO-C, has been well applied in converter, electric furnace, ladle furnace refining and the like. 制造镁碳砖所用到的结合剂一般为酚醛树月旨,酚醛树脂是由酚类和醛类缩聚反应而成,一般情况下用苯酚和甲醛为原材料,由于苯酚价格偏高直接造成了酚醛树脂的成本较高,价格15000元/吨。 The manufacturing MgO-C binding agent used is generally dated purpose phenolic resin, the phenolic resin is a polycondensation reaction from phenols and aldehydes, with phenol and formaldehyde as raw materials in general, as a direct result of the high price of phenol novolac resin the high cost, the price of 15,000 yuan / ton. 虽然市场上普通的酚醛树脂制造的镁碳砖质量较好,但由于普通酚醛树脂价格的偏高,也制约了镁碳砖的快速发展, 因此开发一种低成本的镁碳砖用酚醛树脂是十分必要的。 While better quality MgO-C ordinary phenolic resin manufactured on the market, but because of the high price of ordinary phenolic resin, also restricted the rapid development of magnesia carbon bricks, so the development of a low-cost Bricks is a phenolic resin very necessary.

发明内容 SUMMARY

[0004] 本发明针对不足,提出一种镁碳砖用酚醛树脂的制备方法,采用得到的酚醛树脂造出的镁碳砖具有良好的机械性能,同时大幅度地降低生产成本。 [0004] The present invention is directed insufficient, MgO-C to provide a preparation method of a phenol resin, a phenol resin obtained using the create Bricks having good mechanical properties, while significantly reducing the cost of production.

[0005] 为了实现上述发明目的,本发明提供以下技术方案:一种镁碳砖用酚醛树脂的制备方法,包括以下步骤: [0005] In order to achieve the above object, the present invention provides the following technical solutions: A method for preparing a phenolic resin MgO-C, comprising the steps of:

[0006] ①、将苯酚、甲醛和碱性催化剂按物质的量比1.0 : 1.1〜1.5 : 0.01〜0.03加 [0006] ①, phenol, formaldehyde and a basic catalyst is 1.0 ratio of: 1.1~1.5: 0.01~0.03 plus

入反应釜中,升温至60〜90°C,恒温1〜4小时; Into the reaction vessel, warmed to 60~90 ° C, the thermostat 1 ~ 4 hours;

[0007] ②、向反应釜中加入占苯酚重量10〜20%的造纸废液和2〜5%的醇类物质,搅拌均勻; [0007] ②, paper waste accounts for 10-20% by weight of phenol and alcohols of 2 ~ 5% was added to the reaction vessel, stir;

[0008] ③、60〜90 °C下真空蒸馏步骤②的混勻物,至混勻物的粘度为3000〜 25000MPa · s/25°C。 [0008] ③, ② the step of vacuum distillation at 60~90 ° C was mixed, kneaded to a viscosity of 3000~ 25000MPa · s / 25 ° C.

[0009] 优选的,步骤①中碱性催化剂选自氢氧化钠、氢氧化钙、碳酸钠、氧化钙的一种或多种。 [0009] Preferably, in the step ① basic catalyst selected from sodium hydroxide, calcium hydroxide, sodium carbonate, calcium oxide, one or more.

[0010] 优选的,步骤②中醇类选自二元醇或三元醇。 [0010] Preferably, the step ② the alcohol is selected from dihydric or trihydric alcohols.

[0011] 优选的,所述二元醇为乙二醇或二乙二醇。 [0011] Preferably, the dihydric alcohol is ethylene glycol or diethylene glycol.

[0012] 优选的,所述三元醇为丙三醇。 [0012] Preferably, the triol is glycerol.

[0013] 优选的,步骤③中真空蒸馏的压力为0. 01〜0. 06MPa。 [0013] Preferably, the vacuum distillation step ③ pressure of 0. 01~0. 06MPa.

[0014] 一种镁碳砖用酚醛树脂,采用如上所述的制备方法制备而成。 [0014] A magnesia-carbon brick with a phenolic resin, prepared by the method described above were prepared.

[0015] 一种镁碳砖,由上述的酚醛树脂,与镁砂骨料、镁砂细粉和石墨混勻,成型而制成。 [0015] A MgO-C, with the magnesia aggregate, magnesia and graphite powder by the mixing of a phenolic resin, molding is made. [0016] 与现有技术相比,本发明向常规方法制备的酚醛树脂中加入造纸废液和醇类物质,其中由于造纸废液中30〜50wt%的为木质素,而木质素具有与酚醛树脂相似的结构, 因此可以部分替代苯酚用于酚醛树脂的生产。 [0016] Compared with the prior art, the present invention is a phenol resin prepared by a conventional method was added to the paper waste and alcohols, in which the paper waste due 30~50wt% of the lignin, while the lignin with a phenol resin similar structure, and therefore can partially substitute for the phenol novolac resin production. 在酚醛树脂体系中加入造纸废液后,在碱性环境下,木质素的活性点数目在一定程度上有所增加,并进一步参与苯酚与甲醛之间的聚合反应,不但提高了酚醛树脂的固含量和残碳率,而且在一定程度上也提高了酚醛树脂的性价比。 After addition of paper waste phenolic resin system, in an alkaline environment, the number of active points in the lignin has been increased to some extent, and further participate in the polymerization reaction between phenol and formaldehyde, not only improves the solid phenol resin content and residual carbon ratio, and to some extent also increased cost phenolic resin. 而加入的醇类物质,用来调节所制备的酚醛树脂的粘度;由于一元醇的沸点较低, 本发明使用的为高沸点的二元醇或三元醇。 Added for alcohols, used to adjust the viscosity of the phenolic resin produced; lower boiling point of the monohydric alcohol, the present invention is used as a high-boiling diol or triol.

[0017] 采用本发明制备的酚醛树脂,与镁砂骨料、镁砂细粉、石墨进行混合,然后成型处理得到的镁碳砖,具有良好的机械性能:耐压强度和高温抗折强度,同时由于本发明酚醛树脂的制作成本低,从而能大幅度地降低镁碳砖的生产成本。 [0017] The phenol resin prepared according to the present invention, with the magnesia aggregate, magnesia powder, mixing graphite and MgO-C molding process obtained, having good mechanical properties: compressive strength and high temperature flexural strength, low production cost and because the phenol resin of the present invention, which can greatly reduce the production cost strenth.

具体实施方式 detailed description

[0018] 下面结合具体实施例对本发明进行详细描述,本部分的描述仅是示范性和解释性,不应对本发明的保护范围有任何的限制作用。 [0018] Specific embodiments of the present invention in conjunction with the following detailed description, is described in this section merely exemplary and explanatory, the scope of the present invention should not have any limiting effect.

[0019] 实施例1 [0019] Example 1

[0020] 将苯酚、甲醛、氢氧化钠按物质的量比1 : 1.5 : 0.01加入反应釜中,加热搅拌至60 V,在此温度范围内恒温4小时后,60 V加入苯酚重量20 %的造纸废液,恒温3小时后,加入苯酚重量3%的乙二醇,60°C和0. OlMPa下脱水至树脂粘度为4300MPa · s/25°C。 [0020] phenol, formaldehyde, sodium hydroxide by the molar ratio 1: 1.5: 0.01 added to the kettle and heated with stirring to 60 V, at constant temperature within this temperature range after 4 hours, 60 V was added 20% by weight of phenol paper waste, after constant for 3 hours, and phenol was added 3% by weight of ethylene glycol, 60 ° C and dewatered to 0. OlMPa resin viscosity 4300MPa · s / 25 ° C.

[0021 ] 本实施例生产出的酚醛树脂固含量为75〜82 %,残碳率为45〜48 %,水分为4〜 6%,游离酚为7〜10%。 [0021] The present embodiment produces the phenolic resin solids content of 75~82%, a residual carbon rate of 45~48%, a water content of 4 ~ 6%, 7 to 10% of free phenol.

[0022] 实施例2 [0022] Example 2

[0023] 将苯酚、甲醛、氢氧化钙按物质的量比1 : 1.3 : 0.02加入反应釜中,加热搅拌至700C,在此温度范围内恒温3小时后,70°C加入苯酚重量10%的造纸废液,恒温2小时后,力口入苯酚重量2%的丙三醇,70°C和0. 06MPa下真空脱水至树脂粘度为IOOOOmPa · s/25°C。 [0023] phenol, formaldehyde, calcium hydroxide by molar ratio 1: 1.3: 0.02 added to the kettle and heated to 700C with stirring, the temperature in this temperature range for three hours, 70 ° C was added 10% by weight of phenol paper waste, constant-temperature two hours, force mouth phenol 2 weight% glycerol, 70 ° C and dehydrated under vacuum to 0. 06MPa resin viscosity IOOOOmPa · s / 25 ° C.

[0024] 本实施例生产出的酚醛树脂固含量为76〜83%,残碳率为45〜50%,水分为4〜 6%,游离酚为7〜10%。 [0024] The present embodiment produces the phenolic resin solids content of 76~83%, a residual carbon rate of 45~50%, a water content of 4 ~ 6%, 7 to 10% of free phenol.

[0025] 实施例3 [0025] Example 3

[0026] 将苯酚、甲醛、氢氧化钠按物质的量比1 : 1. 1 : 0.03加入反应釜中,加热搅拌至80°C,在此温度范围内恒温2小时后,80°C加入苯酚重量15%的造纸废液,恒温1小时后,力口入苯酚重量5%的二乙二醇,80°C和0. 04MPa下真空脱水至树脂粘度为7000MPa · s/25°C。 [0026] phenol, formaldehyde, sodium hydroxide by the molar ratio 1: 1.1: 0.03 added to the kettle and heated with stirring to 80 ° C, at a constant temperature within this temperature range after 2 hours, 80 ° C was added phenol 15% by weight of the paper waste, the constant temperature for 1 hour phenol force mouth 5% by weight of diethylene glycol, 80 ° C and dehydrated under vacuum to 0. 04MPa resin viscosity 7000MPa · s / 25 ° C.

[0027] 本实施例生产出的酚醛树脂固含量为75〜83 %,残碳率为45〜49 %,水分为4〜 6%,游离酚为7〜10%。 [0027] The present embodiment produces the phenolic resin solids content of 75~83%, a residual carbon rate of 45~49%, a water content of 4 ~ 6%, 7 to 10% of free phenol.

[0028] 对比实施例 [0028] Comparative Example

[0029] 将上述实施例1、实施例2或实施例3所制得的酚醛树脂与市场上普通的酚醛树月旨,分别作为煤炭装的结合剂,与镁砂骨料、镁砂细粉、石墨等制砖原料混合后压制成砖坯, 再经加热干燥制成镁碳砖,进行对比实验,结果见表1和表2。 [0029] The above-described Example 1, Example 2 or the embodiment of a phenolic resin prepared in Example Market 3 months a normal purpose phenolic resin, respectively, as a binding agent loaded coal, aggregate and magnesia, magnesia powder , graphite brick after the mixed raw material pressed into brick, made of MgO-C and then dried by heating, comparative tests, the results shown in table 1 and table 2.

[0030] 表1镁碳砖的成分 [0030] Table 1 component strenth

Figure CN102127197AD00051

[0032] 表2不同结合剂的镁碳砖对比试验结果 [0032] Table 2 Comparative MgO-C Test results of different binding agents

[0033] [0033]

Figure CN102127197AD00052

[0034] [0034]

[0035] 由表1可以看出,上述镁碳砖只是结合剂不同,其他组分、含量都一样;对这四组镁碳砖进行对比检测试验,所得结果由表2列出。 [0035] As can be seen from Table 1, magnesia-carbon brick above but different binding agents, the other components are the same contents; these four groups were compared MgO-C testing, the results listed in Table 2. 由表2结果可知,在制砖条件相同的情况下,本发明的所生产的镁碳砖和普通酚醛树脂所生产的镁碳砖检测结果相似,即能维持原良好的性能,但成本大大降低。 Table 2 shows the results, under the same conditions are brick, produced according to the present invention Bricks ordinary phenol resin and produced Bricks similar detection results, i.e., to maintain the original excellent performance, but greatly reduce the cost . 由于普通酚醛树脂价格15000元/吨,而本发明的酚醛树脂由于采用造纸废液进行废物利用,成本价格为13000元/吨。 Since ordinary phenol resin price 15,000 yuan / ton, while the phenol resin of the present invention since using paper waste for recycling, the cost price of 13,000 yuan / ton.

[0036] 以上仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。 [0036] The above are only preferred embodiments of the present invention, it should be noted that those of ordinary skill in the art, in the present invention without departing from the principles of the premise, can make various improvements and modifications, improvements and modifications of these also it is considered the scope of the present invention.

Claims (8)

  1. 1. 一种镁碳砖用酚醛树脂的制备方法,包括以下步骤:①、将苯酚、甲醛和碱性催化剂按物质的量比1.0 : 1.1〜1.5 : 0.01〜0.03加入反应釜中,升温至60〜90°C,恒温1〜4小时;②、向反应釜中加入占苯酚重量10〜20%的造纸废液和2〜5%的醇类物质,搅拌均勻;③、60〜90 °C下真空蒸馏步骤②的混勻物,至混勻物的粘度为3000〜 25000MPa · s/25°C。 1. A method for preparing a phenolic resin MgO-C, comprising the steps of: ①, phenol, formaldehyde and a basic catalyst is 1.0 ratio of: 1.1~1.5: 0.01~0.03 added to the kettle and heated to 60 ~90 ° C, temperature ~ 4 hours; ②, by weight of phenol was added paper waste accounts for 10-20% of 2 ~ 5% of alcohols and to the kettle, uniformly stirred; ③, at 60~90 ° C ② the vacuum distillation step was mixed, kneaded to a viscosity of 3000~ 25000MPa · s / 25 ° C.
  2. 2.如权利要求1所述的制备方法,其特征在于:步骤①中碱性催化剂选自氢氧化钠、氢氧化钙、碳酸钠、氧化钙的一种或多种。 The production method as claimed in claim 1, wherein: in the step ① basic catalyst selected from sodium hydroxide, calcium hydroxide, sodium carbonate, calcium oxide, one or more.
  3. 3.如权利要求1所述的制备方法,其特征在于:步骤②中醇类选自二元醇或三元醇。 The production method as claimed in claim 1, wherein: the step ② the alcohol is selected from dihydric or trihydric alcohols.
  4. 4.如权利要求3所述的制备方法,其特征在于:所述二元醇为乙二醇或二乙二醇。 The production method as claimed in claim 3, wherein: the dihydric alcohol is ethylene glycol or diethylene glycol.
  5. 5.如权利要求3所述的制备方法,其特征在于:所述三元醇为丙三醇。 5. The method as recited in claim 3, wherein: said triol is glycerol.
  6. 6.如权利要求1所述的制备方法,其特征在于:步骤③中真空蒸馏的压力为0. 01〜 0.06MPa。 The production method as claimed in claim 1, wherein: the step ③ vacuum distillation pressure of 0. 01~ 0.06MPa.
  7. 7. 一种镁碳砖用酚醛树脂,采用如权利要求1所述的制备方法制备而成。 A magnesia-carbon brick with a phenolic resin, prepared by using the production method according to claim 1.
  8. 8. 一种镁碳砖,由如权利要求7所述的酚醛树脂,与镁砂骨料、镁砂细粉和石墨混勻, 成型而制成。 A MgO-C, the phenolic resin as claimed in claim 7, with the magnesia aggregate, magnesia and graphite powder mix, molding is made.
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CN102276957A (en) * 2011-08-02 2011-12-14 山东圣泉化工股份有限公司 Bricks with a phenolic resin and preparation method
CN103030759A (en) * 2012-12-19 2013-04-10 山东圣泉化工股份有限公司 Lignin phenol resin prepolymer and preparation method thereof, lignin phenol resin and preparation method thereof
CN103183798A (en) * 2011-12-29 2013-07-03 财团法人工业技术研究院 Method for preparing phenol-formaldehyde resins, resin materials and method for preparing resin molding materials
CN104628404A (en) * 2015-03-02 2015-05-20 新乡市熔鑫耐材有限责任公司 Preparation method of carbon-carbon combined refractory material binding agent
CN105503212A (en) * 2015-12-21 2016-04-20 江苏苏嘉集团新材料有限公司 Magnesia carbon brick and preparation method thereof
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CN105670217A (en) * 2016-01-27 2016-06-15 长兴华晨化工有限公司 Production technology of novel special resin for magnesite-dolomite carbon bricks

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CN102276957A (en) * 2011-08-02 2011-12-14 山东圣泉化工股份有限公司 Bricks with a phenolic resin and preparation method
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CN103183798A (en) * 2011-12-29 2013-07-03 财团法人工业技术研究院 Method for preparing phenol-formaldehyde resins, resin materials and method for preparing resin molding materials
CN103183798B (en) * 2011-12-29 2015-07-22 财团法人工业技术研究院 Method for preparing phenol-formaldehyde resins, resin materials and method for preparing resin molding materials
CN103030759B (en) * 2012-12-19 2015-01-14 山东圣泉新材料股份有限公司 Lignin phenol resin prepolymer and preparation method thereof, lignin phenol resin and preparation method thereof
CN103030759A (en) * 2012-12-19 2013-04-10 山东圣泉化工股份有限公司 Lignin phenol resin prepolymer and preparation method thereof, lignin phenol resin and preparation method thereof
CN104628404A (en) * 2015-03-02 2015-05-20 新乡市熔鑫耐材有限责任公司 Preparation method of carbon-carbon combined refractory material binding agent
CN104628404B (en) * 2015-03-02 2016-08-24 新乡市炬能耐材有限公司 One of carbon - carbon bond refractory binders prepared
CN105503212A (en) * 2015-12-21 2016-04-20 江苏苏嘉集团新材料有限公司 Magnesia carbon brick and preparation method thereof
CN105503212B (en) * 2015-12-21 2018-07-20 江苏苏嘉集团新材料有限公司 Species MgO-C and its preparation method
CN105670217A (en) * 2016-01-27 2016-06-15 长兴华晨化工有限公司 Production technology of novel special resin for magnesite-dolomite carbon bricks

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