CN108018035A - 一种耐剪切低浓度瓜胶锆冻胶压裂液 - Google Patents
一种耐剪切低浓度瓜胶锆冻胶压裂液 Download PDFInfo
- Publication number
- CN108018035A CN108018035A CN201610934383.9A CN201610934383A CN108018035A CN 108018035 A CN108018035 A CN 108018035A CN 201610934383 A CN201610934383 A CN 201610934383A CN 108018035 A CN108018035 A CN 108018035A
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- China
- Prior art keywords
- fracturing fluid
- guar gum
- zirconium
- agent
- resistant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000012530 fluid Substances 0.000 title claims abstract description 105
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910052726 zirconium Inorganic materials 0.000 title claims abstract description 51
- 238000010008 shearing Methods 0.000 title claims abstract description 39
- 229920002907 Guar gum Polymers 0.000 title claims abstract description 37
- 239000000665 guar gum Substances 0.000 title claims abstract description 37
- 229960002154 guar gum Drugs 0.000 title claims abstract description 37
- 235000010417 guar gum Nutrition 0.000 title claims abstract description 37
- -1 carboxy-methyl hydroxy propyl Chemical group 0.000 claims abstract description 42
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 34
- 229920013818 hydroxypropyl guar gum Polymers 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 18
- 239000000654 additive Substances 0.000 claims abstract description 15
- 238000000518 rheometry Methods 0.000 claims abstract description 15
- 239000004971 Cross linker Substances 0.000 claims abstract description 14
- 230000000996 additive effect Effects 0.000 claims abstract description 14
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003002 pH adjusting agent Substances 0.000 claims abstract description 12
- 239000004927 clay Substances 0.000 claims abstract description 11
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 claims abstract description 10
- 239000003381 stabilizer Substances 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 239000004202 carbamide Substances 0.000 claims abstract description 7
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002585 base Substances 0.000 claims description 25
- 238000004132 cross linking Methods 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 13
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 12
- 230000000855 fungicidal effect Effects 0.000 claims description 7
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- 238000003756 stirring Methods 0.000 claims description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- OKIZCWYLBDKLSU-UHFFFAOYSA-M N,N,N-Trimethylmethanaminium chloride Chemical group [Cl-].C[N+](C)(C)C OKIZCWYLBDKLSU-UHFFFAOYSA-M 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 239000004310 lactic acid Substances 0.000 claims description 6
- 235000014655 lactic acid Nutrition 0.000 claims description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 5
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- 235000011121 sodium hydroxide Nutrition 0.000 claims description 5
- 150000003754 zirconium Chemical class 0.000 claims description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical group [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- IQDGSYLLQPDQDV-UHFFFAOYSA-N dimethylazanium;chloride Chemical compound Cl.CNC IQDGSYLLQPDQDV-UHFFFAOYSA-N 0.000 claims description 4
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical group O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
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- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 2
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 239000000908 ammonium hydroxide Substances 0.000 claims description 2
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- RZOBLYBZQXQGFY-HSHFZTNMSA-N azanium;(2r)-2-hydroxypropanoate Chemical compound [NH4+].C[C@@H](O)C([O-])=O RZOBLYBZQXQGFY-HSHFZTNMSA-N 0.000 claims description 2
- NZSLBYVEIXCMBT-UHFFFAOYSA-N chloro hypochlorite;zirconium Chemical class [Zr].ClOCl NZSLBYVEIXCMBT-UHFFFAOYSA-N 0.000 claims description 2
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- XHFGWHUWQXTGAT-UHFFFAOYSA-N dimethylamine hydrochloride Natural products CNC(C)C XHFGWHUWQXTGAT-UHFFFAOYSA-N 0.000 claims description 2
- AVTYONGGKAJVTE-OLXYHTOASA-L potassium L-tartrate Chemical compound [K+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O AVTYONGGKAJVTE-OLXYHTOASA-L 0.000 claims description 2
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- 150000003839 salts Chemical class 0.000 claims description 2
- HELHAJAZNSDZJO-OLXYHTOASA-L sodium L-tartrate Chemical compound [Na+].[Na+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O HELHAJAZNSDZJO-OLXYHTOASA-L 0.000 claims description 2
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- 239000001509 sodium citrate Substances 0.000 claims description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 2
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- 235000011004 sodium tartrates Nutrition 0.000 claims description 2
- YMBCJWGVCUEGHA-UHFFFAOYSA-M tetraethylammonium chloride Chemical compound [Cl-].CC[N+](CC)(CC)CC YMBCJWGVCUEGHA-UHFFFAOYSA-M 0.000 claims description 2
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims description 2
- NAVWVHRQSDHCHD-UHFFFAOYSA-N 2-hydroxypropane-1,2,3-tricarboxylic acid;potassium Chemical compound [K].OC(=O)CC(O)(C(O)=O)CC(O)=O NAVWVHRQSDHCHD-UHFFFAOYSA-N 0.000 claims 1
- JQLZABHNCZQFNR-UHFFFAOYSA-J O.[Cl-].[Cl-].[Cl-].[Cl-].Cl.Cl.[Zr+4] Chemical compound O.[Cl-].[Cl-].[Cl-].[Cl-].Cl.Cl.[Zr+4] JQLZABHNCZQFNR-UHFFFAOYSA-J 0.000 claims 1
- NQMRYBIKMRVZLB-UHFFFAOYSA-N methylamine hydrochloride Chemical compound [Cl-].[NH3+]C NQMRYBIKMRVZLB-UHFFFAOYSA-N 0.000 claims 1
- 230000001954 sterilising effect Effects 0.000 claims 1
- 238000004659 sterilization and disinfection Methods 0.000 claims 1
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims 1
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- 244000303965 Cyamopsis psoralioides Species 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
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- GZCGUPFRVQAUEE-KVTDHHQDSA-N aldehydo-D-mannose Chemical group OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)C=O GZCGUPFRVQAUEE-KVTDHHQDSA-N 0.000 description 2
- QDMRQDKMCNPQQH-UHFFFAOYSA-N boranylidynetitanium Chemical compound [B].[Ti] QDMRQDKMCNPQQH-UHFFFAOYSA-N 0.000 description 2
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/66—Compositions based on water or polar solvents
- C09K8/68—Compositions based on water or polar solvents containing organic compounds
- C09K8/685—Compositions based on water or polar solvents containing organic compounds containing cross-linking agents
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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Abstract
本发明公开了一种耐剪切低浓度瓜胶锆冻胶压裂液，其组分组成中至少含有以下重量百分数的组分：羧甲基羟丙基瓜胶0.2～0.6％，粘土稳定剂0.1%～0.4%，助排剂0.2%～0.4%，交联剂0.2%～0.4%，流变调节剂0.1%～0.3%，pH调节剂，pH调节剂量为使压裂液的pH保持在10～12；余量为水。所述流变调节剂选自尿素、硫脲。本发明通过加入流变调节剂，控制羧甲基羟丙基瓜胶与有机锆交联剂的交联速率，可以提高锆冻胶压裂液在高剪切下的稳定性能。本发明的耐剪切低浓度瓜胶锆冻胶压裂液，使用浓度低，可耐高剪切，悬砂性能好，使用温度小于170℃。
Description
技术领域
本发明涉及一种耐剪切低浓度瓜胶锆冻胶压裂液，可用做油田开发中水力压裂增产措施的工作液。
背景技术
水力压裂是利用地面高压泵组，以超过地层吸收能力的排量将高粘液体(压裂液)泵入井内，在井底憋起高压，当该压力克服井壁附近地应力达到岩石抗张强度后，就在井底产生裂缝。继续注入带有支撑剂的压裂液，裂缝继续延伸，支撑剂在裂缝中充填。停泵后，由于支撑剂对裂缝的支撑作用，可在地层中形成足够长、有一定导流能力的填砂裂缝。油气井的水力压裂增产技术是改造油气层的有效方法，是油气井、水井增产、增注的有效措施。此技术已经积累了50多年的经验，被广泛应用于油田勘探开发中。
目前应用最广泛的压裂液体系是以瓜胶及其衍生物为增稠剂的压裂液体系，通过增稠剂与交联剂交联形成冻胶，携带支撑剂进入人工裂缝。该体系具有成本低、交联稳定性好、交联可控、耐温性好、现场施工简单、系统配套完善等特点。
常规的瓜胶压裂液在压裂施工过程中会在裂缝中和裂缝壁面残留大量残渣，造成储层伤害，导致地层渗流能力降低和产能下降，直接影响压裂效果。降低增稠剂用量将减少进入地层的固相物质含量，可有效降低压裂液滤液和残渣对裂缝及储层的伤害。但降低瓜尔胶浓度又会遇到压裂液成胶和耐温、抗剪切不稳定，导致冻胶体系黏弹性降低、支撑剂沉降的问题。
瓜胶是一种天然半乳甘露聚糖，属于非离子型高分子，相对分子质量约200×104。在结构上，以β-1,4键相互连接的D-甘露糖单元为主链，不均匀地在主链的一些D-甘露糖单元的C6位上再连接了单个D-半乳糖(β-1,6键)为支链，其半乳糖与甘露糖之比约为1∶1.8。目前用于压裂的瓜胶增稠剂包括：羟丙基瓜胶(HPG)、羧甲基瓜胶(CMG)和羧甲基羟丙基瓜胶(CMHPG)，其使用浓度一般在0.2～0.8％。
常用交联剂包括硼类交联剂和过渡金属交联剂。硼类交联剂主要包括硼砂、硼酸，及硼与络合剂组成的混合物等，其主要特点是交联可逆、耐高剪切，主要缺点是不耐高温(一般使用温度小于130℃)。过渡金属交联剂主要包括有机锆交联剂和有机钛交联剂，其主要特点是化学交联、耐高温，可以作为低浓度瓜胶压裂液的交联剂使用，但其主要问题是不耐高剪切、交联过程不可逆。
美国专利US6017855提出用乳酸锆交联剂交联羧甲基瓜胶形成低浓度瓜胶压裂液的方法，所使用的羧甲基瓜胶或羧甲基羟丙基瓜胶水溶液的临界交叠浓度小于0.06％，当瓜胶浓度为0.24％时，体系耐温达到105℃。
美国专利US 6214773提出用羧甲基羟丙基瓜胶和有机硼钛交联剂形成压裂液的方法，压裂液体系中羧甲基羟丙基瓜胶浓度为0.12～0.48％，有机硼钛延迟交联剂浓度为0.04～1％，破胶剂0.01～2.5％，压裂液体系适用温度为50～135℃。
美国专利US 8034750提出用羧甲基羟丙基瓜胶与有机硼锆交联剂形成压裂液的方法，压裂液中羧甲基羟丙基瓜胶浓度为0.48％～0.60％，有机硼锆交联剂为烷氧基锆与硼酸形成的混合物，使用浓度为0.1％～0.2％，体系耐温150～170℃。
中国专利CN 101633840B中采用疏水改性的羧甲基羟丙基瓜胶作为增稠剂，有机锆作为交联剂，制备了可耐高温的瓜胶压裂液冻胶。其增稠剂是多烷氧基胺疏水基团接枝的羧甲基瓜胶，交联剂是四(2-羟丙基)乙二胺锆或乳酸锆，适用温度50～190℃，体系中增稠剂浓度为0.15～0.60％，该体系具有瓜胶使用浓度低、摩阻低、耐高温等特点。
羧甲基羟丙基瓜胶锆冻胶压裂液具有瓜胶使用浓度低、对储层伤害小、耐温性好等特点，可以用于高温低渗透储层压裂施工，但由于其剪切不可回复的特性，通常需要在交联剂中加入硼酸。有必要提供另外一种提高羧甲基羟丙基瓜胶锆冻胶耐高剪切的方法。
发明内容
针对上述现有技术，本发明提供了一种耐剪切低浓度瓜胶锆冻胶压裂液(羧甲基羟丙基瓜胶和有机锆交联剂及其他添加剂形成冻胶压裂液)，采用可释放碱的物质作为压裂液的流变调节剂，从而可有效提高羧甲基羟丙基瓜胶锆冻胶的耐高剪切性能。
本发明是通过以下技术方案实现的：
一种耐剪切低浓度瓜胶锆冻胶压裂液，其组分组成中至少含有以下重量百分数的组分：羧甲基羟丙基瓜胶0.2～0.6％，粘土稳定剂0.1％～0.4％，助排剂0.2％～0.4％，交联剂0.2％～0.4％，流变调节剂0.1％～0.3％，pH调节剂，pH调节剂量为使压裂液的pH保持在10～12；余量为水。除此之外，还可含有压裂液中常见的破乳剂、消泡剂、杀菌剂等添加剂。另外，在一些需要交联延迟的情况下，还可以适当地添加交联延迟剂来使交联时间延长。
所述羧甲基羟丙基瓜胶为现有技术中的产品，可常规市场购买得到，本发明所用购自山东广浦生物科技有限公司，其羧甲基取代度大于0.15，羟丙基取代度大于0.15，含水率小于10％，0.6％水溶液表观粘度大于111mPa·s，水不溶物小于4.0％。
所述粘土稳定剂选自小分子季铵盐化合物，包括四甲基氯化铵、四乙基氯化铵、甲胺盐酸盐、二甲胺盐酸盐、三甲胺盐酸盐中的任一种。
所述助排剂选自胜利油田工程院提供的微乳液助排剂，商品名为ME-1.该微乳液助排剂由如下质量份％配比的原料组成：
双子表面活性剂 20～40 非离子表面活性剂 3～4
助表面活性剂 40～60 水 余量。
所述双子表面活性剂为乙撑基双烷基二甲基氯化铵、丙撑基双烷基二甲基氯化铵、乙撑基双烷基二甲基溴化铵或丙撑基双烷基二甲基溴化铵。所述乙撑基双烷基二甲基氯化铵、丙撑基双烷基二甲基氯化铵、乙撑基双烷基二甲基溴化铵或丙撑基双烷基二甲基溴化铵中的烷基可以是十二烷基、十四烷基、十六烷基或十八烷基的任意一种。
所述非离子表面活性剂为椰子油脂肪酸单乙醇酰胺、椰子油脂肪酸二乙醇酰胺、月桂酸单乙醇酰胺或月桂酸二乙醇酰胺。
所述助表面活性剂为乙醇、正丙醇、异丙醇或异丁醇。
该微乳液助排剂的制备方法按如下步骤进行：
a.先将10～20质量份水加入反应器中，再将40～60质量份的助表面活性剂加入水中，室温下搅拌至完全溶解；
b.取20～40质量份双子表面活性剂及3～4质量份非离子表面活性剂依次加入反应器中，补充水至反应器内混合物为100质量份，室温下搅拌均匀，得产品。
所述交联剂选自有机锆交联剂或水基锆交联剂，有机锆交联剂包括四(正丙基)锆酸酯、四(三乙醇胺)锆酸酯、四乳酸锆酸酯、乳酸三(三乙醇胺)锆酸酯。
所述水基锆交联剂，是由无机锆盐与羟基羧酸盐反应形成的络合物，其中，无机锆盐选自氧氯化锆或四氯化锆，羟基羧酸盐选自乳酸钠、乳酸铵、乳酸钾、柠檬酸钠、柠檬酸铵、柠檬酸钾、天冬氨酸钠、酒石酸钠、酒石酸钾等；制备时，无机锆盐与羟基羧酸盐在水中混合均匀，再添加多羟基化合物(如丙三醇)，60～80℃条件下加热2h后制得。
所述流变调节剂选自可以延迟释放碱的化合物，包括尿素、硫脲。
所述pH调节剂选自碱性化合物，包括氢氧化钠、氢氧化钾、碳酸钠、碳酸钾。
所述杀菌剂选自可以抑制压裂液中细菌生长的化合物，包括甲醛、乙醛、戊二醛。
所述交联延迟剂选自碳酸氢钾、碳酸氢钠。
所述耐剪切低浓度瓜胶锆冻胶压裂液的制备方法为：将各组分混合，混匀，即得。
本发明的耐剪切低浓度瓜胶锆冻胶压裂液，通过加入流变调节剂，在压裂液体系中控制羧甲基羟丙基瓜胶与有机锆交联剂的交联速率，可以提高锆冻胶压裂液在高剪切下的稳定性能。本发明的耐剪切低浓度瓜胶锆冻胶压裂液，使用浓度低，可耐高剪切，悬砂性能好，使用温度小于170℃。
附图说明
图1：压裂液耐温耐剪切性能(140℃)(实施例4)。
图2：压裂液在高剪切条件下的耐温耐剪切性能(140℃)(实施例4)。
图3：压裂液在高剪切条件下的耐温耐剪切性能(140℃)(实施例5)。
图4：压裂液耐温耐剪切性能(120℃)(实施例7)。
图5：压裂液耐温耐剪切性能(160℃)(实施例9)。
图6：压裂液静态悬砂性能对比，其中，(1)0h；(2)4h；(3)24h；(4)96h。
具体实施方式
下面结合实施例对本发明作进一步的说明。
下述实施例中所涉及的仪器、试剂、材料等，若无特别说明，均为现有技术中已有的常规仪器、试剂、材料等，可通过正规商业途径获得。下述实施例中所涉及的实验方法，检测方法等，若无特别说明，均为现有技术中已有的常规实验方法，检测方法等。
实施例1 制备有机锆交联剂四(三乙醇胺)锆酸酯
取12g锆酸四正丙酯加入三口烧瓶，开始搅拌，加入7.5g三乙醇胺和7.5g正丙醇，加热到60℃，反应2h；加热过程中，产生白色固体；加入1g水后固体溶解，再加热到80℃，反应4h，得到黄色液体，含锆12％。
实施例2 制备水基锆交联剂(锆与络合剂在水中形成多核羟桥结构)
取10g氧氯化锆加入三口烧瓶，同时加入40g水，搅拌溶解。将12g乳酸加入13g氨水中混合均匀，再将此混合物滴加到烧瓶中，最后加入甘油4g，升温至60℃，反应2h后得到无色液体，含锆3.57％。
实施例3 配制压裂液基液
在混调器中加入494g水，在搅拌下加入2.25g羧甲基羟丙基瓜胶，溶解3min后，依次加入2.5g粘土稳定剂四甲基氯化铵、1.5g微乳液助排剂(ME-1)、0.1g氢氧化钠、0.05g杀菌剂甲醛，搅拌溶解2min，放置1h，配制成羧甲基羟丙基瓜胶浓度为0.45％的压裂液基液。压裂液基液表观粘度70mPa·s(170s-1)，pH值为10.5。
实施例4 压裂液交联性能和耐温耐剪切性能
取实施例3配制的压裂液基液100mL，加入实施例2制备的水基锆交联剂0.3g，得到羧甲基羟丙基锆冻胶压裂液，交联时间2min。采用SY/T 5107-2005《水基压裂液性能评价方法》中规定的压裂液耐温耐剪切测试方法，用HAAKE MARS III高温流变仪测试了140℃条件下压裂液的耐温耐剪切性能。140℃、170s-1条件下剪切90min体系表观粘度为202mPa·s。实验结果如图1所示。
测试该压裂液在高剪切条件下的稳定性，具体方法是：取上述压裂液48mL加入流变仪中，在30℃、1350s-1条件下剪切5min，再降低至170s-1，升温至140℃剪切90min，最终体系表观粘度为52mPa·s，且实验结束后冻胶变成碎块。实验结果如图2所示。
此例说明羧甲基羟丙基瓜胶锆冻胶压裂液在高剪切条件下的耐温耐剪切能力不佳。
实施例5 压裂液交联性能和耐温耐剪切性能
取实施例3配制的压裂液基液100mL，加入0.1g流变调节剂尿素，再加入实施例2制备的水基锆交联剂0.3g，得到羧甲基羟丙基锆冻胶压裂液，交联时间2min。测试该压裂液在高剪切条件下的稳定性，具体方法是：取上述压裂液48mL加入流变仪中，在30℃、1350s-1条件下剪切5min，再降低至170s-1，升温至140℃剪切90min，最终体系表观粘度为150mPa·s，且实验结束后冻胶整体性好。实验结果如图3所示。
此例说明添加流变调节剂后压裂液体系耐高剪切能力提高。
实施例6 配制压裂液基液
在混调器中加入495g水，在搅拌下加入1.5g羧甲基羟丙基瓜胶，溶解3min后，依次加入2.5g粘土稳定剂四甲基氯化铵、1.5g助排剂ME-1、0.1g氢氧化钠、0.05g杀菌剂甲醛，搅拌溶解2min，放置1h，配制成羧甲基羟丙基瓜胶浓度为0.30％的压裂液基液。压裂液基液表观粘度33mPa·s(170s-1)，pH值为10.5。
实施例7 压裂液交联性能和耐温耐剪切性能
取实施例6配制的压裂液基液100mL，加入0.1g流变调节剂尿素，加入实施例2制备的水基锆交联剂0.3g，得到羧甲基羟丙基锆冻胶压裂液，交联时间3min。采用SY/T5107-2005《水基压裂液性能评价方法》中规定的压裂液耐温耐剪切测试方法，用HAAKE MARS III高温流变仪测试了120℃条件下压裂液的耐温耐剪切性能。120℃、170s-1条件下剪切90min体系表观粘度大于300mPa·s。实验结果见图4所示。
实施例8 配制压裂液基液
在混调器中加入493g水，在搅拌下加入3g羧甲基羟丙基瓜胶，溶解3min后，依次加入2.5g粘土稳定剂四甲基氯化铵、1.5g助排剂ME-1、0.1g氢氧化钠、0.05g杀菌剂甲醛，搅拌溶解2min，放置1h，配制成羧甲基羟丙基瓜胶浓度为0.60％的压裂液基液。压裂液基液表观粘度111mPa·s(170s-1)，pH值为10.5。
实施例9 压裂液交联性能和耐温耐剪切性能
取实施例8配制的压裂液基液100mL，加入0.1g流变调节剂尿素，加入实施例1制备的有机锆交联剂0.3g，得到羧甲基羟丙基锆冻胶压裂液，交联时间1min。采用SY/T5107-2005《水基压裂液性能评价方法》中规定的压裂液耐温耐剪切测试方法，用HAAKE MARS III高温流变仪测试了160℃条件下压裂液的耐温耐剪切性能。160℃、170s-1条件下剪切90min体系表观粘度为124mPa·s。实验结果见图5所示。
实施例10 静态悬砂性能
以常规羟丙基瓜胶硼冻胶和羧甲基羟丙基瓜胶锆冻胶为对比，对比了两者的静态悬砂性能。常规羟丙基瓜胶硼冻胶压裂液中瓜胶浓度为0.60％，有机硼交联剂浓度为0.30％，羧甲基羟丙基瓜胶锆冻胶为实施例5配制的压裂液，支撑剂采用Carbo Prop30/60陶粒，实验砂比20％，实验结果见图6。
实验结果说明，羧甲基羟丙基瓜胶锆冻胶的静态悬砂性能优异。
实施例11 现场应用
义283井位于济阳坳陷沾化凹陷渤南洼陷义107井区鼻状构造带义283构造较高部位。改造层段(3650～3760m)碳酸盐岩含量为45％～65％，砂质岩含量为15％～20％，粘土含量为15％～25％，脆性矿物含量大于70％。孔隙度为5％～7％，含油饱和度平均为50％～70％。地层温度145℃，采用瓜胶浓度为0.45％的羧甲基羟丙基锆冻胶压裂液(实施例5制备)进行压裂施工。
现场压裂施工于2015年12月进行，共使用速溶型低浓度瓜胶压裂液1250m3，压裂施工压力58～65MPa，最高砂比30％，总加砂120m3。压裂液现场交联时间3～4min，交联情况良好，顺利完成压裂施工。该井最高日产油22.4t/d，压裂效果显著。
上述虽然结合实施例对本发明的具体实施方式进行了描述，但并非对本发明保护范围的限制，所属领域技术人员应该明白，在本发明的技术方案的基础上，本领域技术人员不需要付出创造性劳动即可做出的各种修改或变形仍在本发明的保护范围以内。
Claims (10)
1.一种耐剪切低浓度瓜胶锆冻胶压裂液，其特征在于：其组分组成中至少含有以下重量百分数的组分：羧甲基羟丙基瓜胶0.2～0.6％，粘土稳定剂0.1％～0.4％，助排剂0.2％～0.4％，交联剂0.2％～0.4％，流变调节剂0.1％～0.3％，pH调节剂，pH调节剂量为使压裂液的pH保持在10～12；余量为水；
所述粘土稳定剂选自四甲基氯化铵、四乙基氯化铵、甲胺盐酸盐、二甲胺盐酸盐、三甲胺盐酸盐中的任一种；
所述助排剂选自微乳液助排剂；
所述交联剂选自有机锆交联剂或水基锆交联剂；
所述流变调节剂选自尿素、硫脲；
所述pH调节剂选自碱性化合物。
2.根据权利要求1所述的耐剪切低浓度瓜胶锆冻胶压裂液，其特征在于：组分中还含有破乳剂、消泡剂、杀菌剂或/和交联延迟剂。
3.根据权利要求2所述的耐剪切低浓度瓜胶锆冻胶压裂液，其特征在于：是由以下重量百分数的组分组成的：羧甲基羟丙基瓜胶0.2～0.6％，粘土稳定剂0.1％～0.4％，助排剂0.2％～0.4％，交联剂0.2％～0.4％，流变调节剂0.1％～0.3％，杀菌剂0.05～0.2％，pH调节剂，pH调节剂量为使压裂液的pH保持在10～12；余量为水。
4.根据权利要求1～3中任一项所述的耐剪切低浓度瓜胶锆冻胶压裂液，其特征在于：所述羧甲基羟丙基瓜胶，羧甲基取代度大于0.15，羟丙基取代度大于0.15，含水率小于10％，0.6％水溶液表观粘度大于111mPa·s，水不溶物小于4.0％。
5.根据权利要求1～3中任一项所述的耐剪切低浓度瓜胶锆冻胶压裂液，其特征在于：所述有机锆交联剂选自四(正丙基)锆酸酯、四(三乙醇胺)锆酸酯、四乳酸锆酸酯、乳酸三(三乙醇胺)锆酸酯。
6.根据权利要求1～3中任一项所述的耐剪切低浓度瓜胶锆冻胶压裂液，其特征在于：所述水基锆交联剂，是由无机锆盐与羟基羧酸盐反应形成的络合物，其中，无机锆盐选自氧氯化锆或四氯化锆，羟基羧酸盐选自乳酸钠、乳酸铵、乳酸钾、柠檬酸钠、柠檬酸铵、柠檬酸钾、天冬氨酸钠、酒石酸钠、酒石酸钾。
7.根据权利要求1～3中任一项所述的耐剪切低浓度瓜胶锆冻胶压裂液，其特征在于：所述pH调节剂选自氢氧化钠、氢氧化钾、碳酸钠、碳酸钾。
8.根据权利要求2或3所述的耐剪切低浓度瓜胶锆冻胶压裂液，其特征在于：所述杀菌剂选自甲醛、乙醛、戊二醛。
9.根据权利要求2或3所述的耐剪切低浓度瓜胶锆冻胶压裂液，其特征在于：所述所述交联延迟剂选自碳酸氢钾、碳酸氢钠。
10.根据权利要求4所述的耐剪切低浓度瓜胶锆冻胶压裂液，其特征在于：是由以下组分组成的：水494g，羧甲基羟丙基瓜胶2.25g，粘土稳定剂四甲基氯化铵2.5g，助排剂ME-11.5g，交联剂0.3g，流变调节剂尿素0.1g，杀菌剂0.05g，pH调节剂，pH调节剂量为使压裂液的pH保持在10.5；
所述交联剂是通过以下方法制备得到的：取10g氧氯化锆加入三口烧瓶，同时加入40g水，搅拌溶解；将12g乳酸加入13g氨水中混合均匀，再将此混合物滴加到三口烧瓶中，最后加入甘油4g，升温至60℃，反应2h后得到无色液体。
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