CN104140788A - 一种钻井液用甲基葡萄糖苷的制备方法 - Google Patents

一种钻井液用甲基葡萄糖苷的制备方法 Download PDF

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CN104140788A
CN104140788A CN201310522827.4A CN201310522827A CN104140788A CN 104140788 A CN104140788 A CN 104140788A CN 201310522827 A CN201310522827 A CN 201310522827A CN 104140788 A CN104140788 A CN 104140788A
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methyl glucoside
acid
drilling fluid
glucose
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司西强
王中华
魏军
甄剑武
万龙
吕跃滨
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China Petroleum and Chemical Corp
Sinopec Oilfield Service Corp
Sinopec Zhongyuan Petroleum Engineering Co Ltd
Drilling Engineering Technology Research Institute of Sinopec Zhongyuan Petroleum Engineering Co Ltd
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Abstract

本发明公开了一种钻井液用甲基葡萄糖苷的制备方法,属油田化学钻井液处理剂技术领域。步骤如下:(1)将葡萄糖与甲醇按摩尔比为1:3~12加入反应瓶,负载质子酸的负载型催化剂按葡萄糖质量的10%~50%加入,在温度60~100℃下搅拌反应3~10h,过滤出负载型催化剂,得到无色透明的反应液,反应完成,即得未处理的甲基葡萄糖苷反应液;(2)将未处理的甲基葡萄糖苷反应液温度降至50℃,用中和剂调节pH值至8.0~10.0,趁热过滤,分离出未反应的葡萄糖,得到脱除葡萄糖的滤液;(3)将脱除葡萄糖的滤液移入单口烧瓶,减压蒸馏除去过量的甲醇,按1:1的体积比加入水,即得到含量为50%的钻井液用甲基葡萄糖苷水溶液。

Description

一种钻井液用甲基葡萄糖苷的制备方法
技术领域
本发明涉及一种钻井液用烷基葡萄糖苷的制备方法,特别是涉及一种钻井液用甲基葡萄糖苷的制备方法,属油田化学钻井液处理剂技术领域。
背景技术
烷基糖苷是利用淀粉或葡萄糖与脂肪醇生产的一类钻井液处理剂,它不仅原料丰富、价廉、而且性能优良、生物降解性好,自上世纪90年代以来逐渐引起了国内外学者的关注,该产品主要应用于日化产品、纺织、皮革助剂、造纸助剂等多个行业。最早将烷基糖苷应用于钻井液的报道出现在1994年在美国达拉斯召开的IADC\SPE钻井工程会议上,研究成果引起了与会者的广泛关注。之后,国内石油大学(北京)和石油大学(华东)及其它研究机构相继开展了相关研究,经过十几年的发展,已取得了一定进展。目前应用于钻井液中的烷基葡萄糖苷主要是甲基葡萄糖苷(MEG)。甲基葡萄糖苷钻井液已经形成比较成熟的体系,有许多成功应用于现场的报道,如在大庆、胜利、辽河、新疆等油田都得到了广泛应用,在中原油田的非常规油气钻井过程中也开始初步应用,如在中原油田的第一口非常规水平井卫383-FP1井上已经成功应用,另外在文88-FP1井和文133-平1井也进行了现场应用,效果较好。专利CN 200910112354.4公开了一种甲基葡萄糖苷的制备方法,以纤维素和甲醇为原料,以甲醇为反应介质,在酸性催化剂存在下,纤维素和甲醇催化反应直接制备甲基葡萄糖苷。整个工艺过程简单,甲基葡萄糖苷的摩尔最高收率可达到65%。目前甲基葡萄糖苷的合成主要采用直接合成法,所用催化剂为无机酸、有机酸或无机酸与有机酸的混合物,催化剂无法回收,且反应过程时间较长,产品收率较低,生产成本较高。
发明内容
本发明的目的是为了克服现有甲基葡萄糖苷制备技术反应时间较长,催化剂无法回收,产品生产成本较高的不足,提供一种反应时间较短,催化剂可回收,生产成本较低的钻井液用甲基葡萄糖苷的制备方法。
甲基葡萄糖苷的具体制备步骤如下:
(1)将葡萄糖与甲醇按摩尔比为1:3~12加入反应瓶,负载质子酸的负载型催化剂按葡萄糖质量的10%~50%加入,在温度60~100℃下搅拌反应3~10h,反应完成,过滤出负载型催化剂,得到无色透明的反应液,即得未处理的甲基葡萄糖苷反应液;
(2)将未处理的甲基葡萄糖苷反应液温度降至40~50℃,用中和剂调节pH值至8.0~10.0,趁热过滤,分离出未反应的葡萄糖,得到脱除葡萄糖的滤液;
(3)将脱除葡萄糖的滤液移入单口烧瓶,减压蒸馏除去过量的甲醇,按1:1的体积比加入水,即得到含量为50%的钻井液用甲基葡萄糖苷水溶液。
所述的中和剂为氢氧化钠、氢氧化钾、碳酸钠中的一种。
所述的负载型催化剂具体制备步骤如下:
(1)将粒径为4~10目的活性炭在300~500℃高温下活化6~10h,制备得到比表面积为700~1500m2/g的负载型催化剂载体;
(2)将质子酸配成质量浓度为10%~30%的水溶液,作为催化剂载体的浸渍液;
(3)将负载型催化剂载体与催化剂载体的浸渍液按质量比为1:2~4混合,浸渍24~48h,得到浸渍后的催化剂;
(4)将浸渍后的催化剂抽滤除去滤液,得到未烘干的负载型催化剂,将未烘干的负载型催化剂在100~110℃下干燥4~8h,制得负载型催化剂。
所述的活性炭为椰壳活性炭、木质活性炭、煤质活性炭中的一种;
所述的质子酸是无机酸、有机酸或无机酸和有机酸的复配的混合物;
所述的无机酸,为硫酸、硝酸、磷酸、盐酸、磷钨酸中的一种;
所述的有机酸,为对甲苯磺酸、十二烷基苯磺酸、氨基磺酸中的一种。
本发明的有益效果是:
本发明采用葡萄糖与甲醇为原料在负载型催化剂催化的条件下制备甲基葡萄糖苷,因为反应过程中以负载型催化剂催化,反应时间较短,催化剂可回收再利用,生产成本较低。
具体实施方式
负载型催化剂制备实施例1
将椰壳活性炭在300℃高温下活化6h,得到负载型催化剂载体;将对甲苯磺酸配成质量浓度为10%的水溶液,制备得到催化剂载体的浸渍液;将负载型催化剂载体与催化剂载体的浸渍液按质量比为1:2混合,浸渍24h,得到浸渍后的催化剂;将浸渍后的催化剂抽滤除去滤液,得到未烘干的负载型催化剂,在100℃下干燥4h,制得制备烷基糖苷的负载型催化剂A。
实施例2~10步骤与实施例1相同,负载型催化剂的具体制备原料用量及制备条件表如表1所示:
表1 负载型催化剂制备原料用量及制备条件表
甲基葡萄糖苷制备实施例1
在装有温度计、冷凝管、分水器的500mL四口烧瓶中,加入葡萄糖180g、甲醇96g和负载型催化剂A 18g,在常压,温度60℃下反应3h,得到无色透明的甲基葡萄糖苷反应液;将滤液温度降至40~50℃,用30%的氢氧化钠溶液调节pH值至8.0,趁热过滤,分离出负载型催化剂A和未反应的葡萄糖,得到脱除葡萄糖的滤液;将脱除葡萄糖的滤液移入单口烧瓶,减压蒸馏除去过量的甲醇,甲基糖苷收率为91.1%,按1:1的体积比加入水,即得到含量为50%的钻井液用甲基葡萄糖苷水溶液。
实施例2~10步骤与实施例1相同,具体反应物质和反应条件如表2所示:
表2 反应物质用量及反应条件表
由表2可知,本发明采用葡萄糖与甲醇为原料在负载型催化剂催化的条件下制备甲基葡萄糖苷,本发明与现有技术相比,反应时间较短,产品收率较高,催化剂可回收再利用,生产成本较低。

Claims (7)

1.一种钻井液用甲基葡萄糖苷的制备方法,其特征在于包括以下步骤:
(1)将葡萄糖与甲醇按摩尔比为1:3~12加入反应瓶,负载质子酸的负载型催化剂按葡萄糖质量的10%~50%加入,在温度60~100℃下搅拌反应3~10h,过滤出负载型催化剂,得到无色透明的反应液,反应完成,即得未处理的甲基葡萄糖苷反应液;
(2)将未处理的甲基葡萄糖苷反应液温度降至40~50℃,用中和剂调节pH值至8.0~10.0,趁热过滤,分离出未反应的葡萄糖,得到脱除葡萄糖的滤液;
(3)将脱除葡萄糖的滤液移入单口烧瓶,减压蒸馏除去过量的甲醇,按1:1的体积比加入水,即得到含量为50%的钻井液用甲基葡萄糖苷水溶液。
2.如权利要求1所述的钻井液用甲基葡萄糖苷的制备方法,其特征在于所述的中和剂为氢氧化钠、氢氧化钾、碳酸钠中的一种。
3.如权利要求1所述的钻井液用甲基葡萄糖苷的制备方法,其特征在于所述的负载型催化剂具体制备步骤如下:
(1)将粒径为4~10目的活性炭在300~500℃高温下活化6~10h,制备得到比表面积为700~1500m2/g的负载型催化剂载体;
(2)将质子酸配成质量浓度为10%~30%的水溶液,作为催化剂载体的浸渍液;
(3)将负载型催化剂载体与催化剂载体的浸渍液按质量比为1:2~4混合,浸渍24~48h,得到浸渍后的催化剂;
(4)将浸渍后的催化剂抽滤除去滤液,得到未烘干的负载型催化剂,将未烘干的负载型催化剂在100~110℃下干燥4~8h,制得负载型催化剂。
4.如权利要求1所述的钻井液用甲基葡萄糖苷的制备方法,其特征在于所述的活性炭为椰壳活性炭、木质活性炭、煤质活性炭中的一种。
5.如权利要求1所述的钻井液用甲基葡萄糖苷的制备方法,其特征在于所述的质子酸是无机酸、有机酸或无机酸和有机酸的复配的混合物。
6.如权利要求1所述的钻井液用甲基葡萄糖苷的制备方法,其特征在于所述的无机酸为硫酸、硝酸、磷酸、盐酸、磷钨酸中的一种。
7.如权利要求1所述的钻井液用甲基葡萄糖苷的制备方法,其特征在于所述的有机酸为对甲苯磺酸、十二烷基苯磺酸、氨基磺酸中的一种。
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CN104388064A (zh) * 2014-10-31 2015-03-04 中国石油化工集团公司 一种氯化钙水基钻井液
CN104388064B (zh) * 2014-10-31 2020-05-22 中国石油化工集团公司 一种氯化钙水基钻井液
CN113512078A (zh) * 2021-07-19 2021-10-19 上海发凯化工有限公司 一种纤维素一锅法直接制备烷基糖苷表面活性剂的方法

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