CN106964399A - 一种异丁烯聚合用催化剂及其制备方法 - Google Patents
一种异丁烯聚合用催化剂及其制备方法 Download PDFInfo
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- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 239000003054 catalyst Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000002808 molecular sieve Substances 0.000 claims abstract description 24
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 24
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 14
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 14
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000011959 amorphous silica alumina Substances 0.000 claims abstract description 10
- 239000011787 zinc oxide Substances 0.000 claims abstract description 10
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 7
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 claims abstract description 7
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 7
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims abstract description 7
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 7
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000292 calcium oxide Substances 0.000 claims abstract description 6
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 6
- 238000009288 screen filtration Methods 0.000 claims description 6
- 239000010457 zeolite Substances 0.000 claims description 6
- 229910021536 Zeolite Inorganic materials 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 3
- 239000000693 micelle Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 230000020477 pH reduction Effects 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 238000010298 pulverizing process Methods 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims 1
- 229910052796 boron Inorganic materials 0.000 claims 1
- 238000006555 catalytic reaction Methods 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- DRHABPMHZRIRAH-UHFFFAOYSA-N 2,4,4,6,6-pentamethylhept-2-ene Chemical group CC(C)=CC(C)(C)CC(C)(C)C DRHABPMHZRIRAH-UHFFFAOYSA-N 0.000 abstract description 6
- FXNDIJDIPNCZQJ-UHFFFAOYSA-N 2,4,4-trimethylpent-1-ene Chemical group CC(=C)CC(C)(C)C FXNDIJDIPNCZQJ-UHFFFAOYSA-N 0.000 abstract description 5
- 239000004615 ingredient Substances 0.000 abstract description 4
- 238000006116 polymerization reaction Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 2
- BZLVMXJERCGZMT-UHFFFAOYSA-N Methyl tert-butyl ether Chemical compound COC(C)(C)C BZLVMXJERCGZMT-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- -1 isobutyls Alkene Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 229910001593 boehmite Inorganic materials 0.000 description 1
- 229920005549 butyl rubber Polymers 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003254 gasoline additive Substances 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/005—Mixtures of molecular sieves comprising at least one molecular sieve which is not an aluminosilicate zeolite, e.g. from groups B01J29/03 - B01J29/049 or B01J29/82 - B01J29/89
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2/00—Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms
- C07C2/02—Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms by addition between unsaturated hydrocarbons
- C07C2/04—Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms by addition between unsaturated hydrocarbons by oligomerisation of well-defined unsaturated hydrocarbons without ring formation
- C07C2/06—Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms by addition between unsaturated hydrocarbons by oligomerisation of well-defined unsaturated hydrocarbons without ring formation of alkenes, i.e. acyclic hydrocarbons having only one carbon-to-carbon double bond
- C07C2/08—Catalytic processes
- C07C2/14—Catalytic processes with inorganic acids; with salts or anhydrides of acids
- C07C2/16—Acids of sulfur; Salts thereof; Sulfur oxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
- B01J2229/186—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself not in framework positions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/72—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing iron group metals, noble metals or copper
- B01J29/76—Iron group metals or copper
- B01J29/7615—Zeolite Beta
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/82—Phosphates
- B01J29/84—Aluminophosphates containing other elements, e.g. metals, boron
- B01J29/85—Silicoaluminophosphates [SAPO compounds]
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- Materials Engineering (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Transition And Organic Metals Composition Catalysts For Addition Polymerization (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
本发明公开了一种异丁烯聚合用催化剂及其制备方法,由以下重量份的物质组成,无定形硅铝10份,分子筛20份,氧化镁13份,碳酸钠9份,活性炭13份,碱性硫酸铝8份,高岭土8份,三氧化二硼17份,三氧化二铁15份,纳米氧化锌颗粒25份,氧化钙8份;本发明采用上述技术方案制备的催化剂具有以下技术效果:采用上述方法制备的催化剂对异丁烯的聚合度具有很好的控制能力,只能将异丁烯定向催化合成为二异丁烯、三异丁烯和四异丁烯;本发明的催化剂对于原料要求较低,适应性强。
Description
技术领域
本发明涉及催化剂技术领域,尤其涉及一种异丁烯聚合用催化剂及其
制备方法。
背景技术
我国拥有丰富的异丁烯资源,它是一种非常好的化工原料,但是目前主要被用来生产附加值较低、需求量巨大的甲基叔丁基醚、叔丁醇、丁基橡胶等,对于异丁烯来说,是一种非常严重的资源浪费。
由于甲基叔丁基醚作为汽油添加剂对水源有潜在污染的风险,已经被美国禁用,导致其生产和应用前景非常不明朗。因此,开发一种新的化工工艺,将异丁烯制备成二异丁烯、三异丁烯和四异丁烯,成为高附加值产品,又解决了异丁烯的去处问题,一举多得。因此,开发一种能够使异丁烯仅仅聚合成为二异丁烯、三异丁烯和四异丁烯,而不产生多聚异丁烯的催化剂就变得很有必要。
发明内容
本发明要解决的技术问题是针对现有技术的不足提供一种异丁烯聚合用聚合催化及其制备方法,采用该方法制备的催化剂对异丁烯的聚合度具有很好的控制能力,只能将异丁烯定向催化合成为二异丁烯、三异丁烯和四异丁烯,对于原料要求较低,适应性强;采用该方法制备的催化剂催化条件温和,反应温度和压力都不高,便于操作,而且经济环保。
为解决上述技术问题本发明采用以下技术方案:一种异丁烯聚合用催化剂,由以下重量份的物质组成,无定形硅铝10份,分子筛20份,氧化镁13份,碳酸钠9份,活性炭13份,碱性硫酸铝8份,高岭土8份,三氧化二硼17份,三氧化二铁15份,纳米氧化锌颗粒25份,氧化钙8份;
所述分子筛为 SAPO-11分子筛与β 沸石分子筛的混合物,SAPO-11分子筛与β沸石分子筛的质量比为1:2;
所述纳米氧化锌颗粒的粒径为 50-10nm,长度为 80-30nm。
所述SAPO-11分子筛的相对结晶度为 98%, 晶体粒径为 2.0μm;
所述无定形硅铝的比表面积为 350 -600m 2 /g,孔容为 0.75 -1.30ml/g。
一种异丁烯聚合用催化剂的制备方法,包括如下步骤:
a、焙烧处理
将无定形硅铝10份,分子筛20份,氧化镁13份,碳酸钠9份,活性炭13份,碱性硫酸铝8份,高岭土8份,三氧化二硼17份,三氧化二铁15份,纳米氧化锌颗粒25份,氧化钙8份混合均匀,送入2000-3000℃的焙烧炉中焙烧8-12小时得到颗粒;
b、酸化步骤;
将上述颗粒加入硝酸0.5mol/l水溶液,碾压成胶团状湿饼后挤条成型,
然后晾晒,晾晒后混合物的含水率≤ 30%。
c、焙烧
将晾晒后的混合物放入焙烧炉中进行焙烧,焙烧温度控制在600-800℃,焙烧时间控制在2小时。
d、将步骤c中焙烧后的混合物进行粉碎处理,然后先用20目的筛网过滤,去除颗粒直径过细的粉末,再将得到的颗粒用10目的筛网过滤,去除颗粒直径过大的部分,得到成品催化剂。
本发明采用上述技术方案制备的催化剂具有以下技术效果:
1、采用上述方法制备的催化剂对异丁烯的聚合度具有很好的控制能力,只能将异丁烯定向催化合成为二异丁烯、三异丁烯和四异丁烯;
2、本发明的催化剂对于原料要求较低,适应性强;
3、本发明的催化剂催化条件温和,反应温度和压力都不高,便于操作,而且经济环保;
4、本发明催化剂能将异丁烯定向催化合成为高附加值的二异丁烯、三异丁烯和四异丁烯,具有很高的经济效益和市场前景;
5、本发明的催化剂对于原料要求较低,因而原料来源广泛,而且原料价格低,保证了产品效益的最大化。
6、本专利催化剂催化反应条件温和,因而单位产品的能耗大大降低,符合国家节能降耗的方针,符合绿色化工的理念。
具体实施方式
实施例,一种异丁烯聚合用催化剂,由以下重量份的物质组成,无定形硅铝10份,分子筛20份,氧化镁13份,碳酸钠9份,活性炭13份,碱性硫酸铝8份,高岭土8份,三氧化二硼17份,三氧化二铁15份,纳米氧化锌颗粒25份,氧化钙8份。
所述分子筛为 SAPO-11分子筛与β 沸石分子筛的混合物,SAPO-11分子筛与β沸石分子筛的质量比为1:2。
所述纳米氧化锌颗粒的粒径为 50-10nm,长度为 80-30nm。
所述SAPO-11分子筛的相对结晶度为 98%, 晶体粒径为 2.0μm。
所述无定形硅铝的比表面积为 350 -600m 2 /g,孔容为 0.75 -1.30ml/g。
所述SAPO-11分子筛的制备方法如下,将90%水溶液的原料磷酸与去离子水混合后搅拌均匀,在搅拌下加入拟薄水铝石,搅拌均匀后再加入含 SiO2 为 25%的硅溶胶,搅拌反应成胶后,最后再将二乙胺溶液和 氢氟酸溶液缓慢加入到上述凝胶中,继续搅拌制成凝胶反应混合物 ;将上述反应混合物装入带有聚四氟乙烯衬套的晶化釜中,在160℃自生压力下晶化 48 小时,最后将晶化产物用去离子水洗涤、过滤,于 100℃空气中烘干,制得SAPO-11 分子筛,相对结晶度为 98%。
一种异丁烯聚合用催化剂及其制备方法,包括如下步骤:
a、焙烧处理
将无定形硅铝10份,分子筛20份,氧化镁13份,碳酸钠9份,活性炭13份,碱性硫酸铝8份,高岭土8份,三氧化二硼17份,三氧化二铁15份,纳米氧化锌颗粒25份,氧化钙8份混合均匀,送入2000-3000℃的焙烧炉中焙烧8-12小时得到颗粒;
b、酸化步骤;
将上述颗粒加入硝酸0.5mol/l水溶液,碾压成胶团状湿饼后挤条成型,
然后晾晒,晾晒后混合物的含水率≤ 30%。
c、焙烧
将晾晒后的混合物放入焙烧炉中进行焙烧,焙烧温度控制在600-800℃,焙烧时间控制在2小时。
d、将步骤c中焙烧后的混合物进行粉碎处理,然后先用20目的筛网过滤,去除颗粒直径过细的粉末,再将得到的颗粒用10目的筛网过滤,去除颗粒直径过大的部分,得到成品催化剂。
Claims (2)
1.一种异丁烯聚合用催化剂,其特征在于:由以下重量份的物质组成,无定形硅铝10份,分子筛20份,氧化镁13份,碳酸钠9份,活性炭13份,碱性硫酸铝8份,高岭土8份,三氧化二硼17份,三氧化二铁15份,纳米氧化锌颗粒25份,氧化钙8份;
所述分子筛为 SAPO-11分子筛与β 沸石分子筛的混合物,SAPO-11分子筛与β沸石分子筛的质量比为1:2;
所述纳米氧化锌颗粒的粒径为 50-10nm,长度为 80-30nm。
2.所述SAPO-11分子筛的相对结晶度为 98%, 晶体粒径为 2.0μm;
所述无定形硅铝的比表面积为 350 -600m 2 /g,孔容为 0.75 -1.30ml/g;
一种异丁烯聚合用催化剂及其制备方法,其特征在于:包括
如下步骤:
a、焙烧处理;
将无定形硅铝10份,分子筛20份,氧化镁13份,碳酸钠9份,活性炭13份,碱性硫酸铝8份,高岭土8份,三氧化二硼17份,三氧化二铁15份,纳米氧化锌颗粒25份,氧化钙8份混合均匀,送入2000-3000℃的焙烧炉中焙烧8-12小时得到颗粒;
b、酸化步骤;
将上述颗粒加入硝酸0.5mol/l水溶液,碾压成胶团状湿饼后挤条成型,
然后晾晒,晾晒后混合物的含水率≤ 30%;
c、焙烧;
将晾晒后的混合物放入焙烧炉中进行焙烧,焙烧温度控制在600-800℃,焙烧时间控制在2小时;
d、将步骤c中焙烧后的混合物进行粉碎处理,然后先用20目的筛网过滤,去除颗粒直径过细的粉末,再将得到的颗粒用10目的筛网过滤,去除颗粒直径过大的部分,得到成品催化剂。
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