CN111215050A - 一种油脂氢化催化剂 - Google Patents
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- 239000003054 catalyst Substances 0.000 title claims abstract description 25
- 238000005984 hydrogenation reaction Methods 0.000 title abstract description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 24
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003921 oil Substances 0.000 claims abstract description 13
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 13
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- 239000002245 particle Substances 0.000 claims abstract description 4
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 6
- 239000003925 fat Substances 0.000 claims 1
- 235000019198 oils Nutrition 0.000 abstract description 12
- 239000007787 solid Substances 0.000 abstract description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 7
- 239000004519 grease Substances 0.000 abstract description 7
- 239000002253 acid Substances 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
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- 230000004913 activation Effects 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 235000010692 trans-unsaturated fatty acids Nutrition 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
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- 229910052759 nickel Inorganic materials 0.000 description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 description 2
- 239000008158 vegetable oil Substances 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
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- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
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- 235000013305 food Nutrition 0.000 description 1
- 235000021588 free fatty acids Nutrition 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 231100000206 health hazard Toxicity 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000008172 hydrogenated vegetable oil Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 235000021281 monounsaturated fatty acids Nutrition 0.000 description 1
- UJVRJBAUJYZFIX-UHFFFAOYSA-N nitric acid;oxozirconium Chemical compound [Zr]=O.O[N+]([O-])=O.O[N+]([O-])=O UJVRJBAUJYZFIX-UHFFFAOYSA-N 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- MUMZUERVLWJKNR-UHFFFAOYSA-N oxoplatinum Chemical compound [Pt]=O MUMZUERVLWJKNR-UHFFFAOYSA-N 0.000 description 1
- 229910003446 platinum oxide Inorganic materials 0.000 description 1
- 235000020777 polyunsaturated fatty acids Nutrition 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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- 239000000126 substance Substances 0.000 description 1
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 1
- 208000001072 type 2 diabetes mellitus Diseases 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/42—Platinum
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
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- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/391—Physical properties of the active metal ingredient
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- B01J35/399—Distribution of the active metal ingredient homogeneously throughout the support particle
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/12—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by hydrogenation
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Abstract
本发明提供一种油脂氢化催化剂，该催化剂由铂负载在ZrO2组成，铂实际负载量为1.79％，其催化剂的比表面积为32.88m2g‑1，比孔容为0.133cm3g‑1，平均孔径为16.16nm，铂粒径大小约为1±0.25nm。本发明制备的催化剂使用浸渍还原法：将六水合氯铂酸配成溶液后与载体浸渍搅拌一段时间后，减压蒸干水分后继续烘干，合成固体煅烧并于纯氢气高温还原制成催化剂。本发明的特点是：催化剂的制备工艺简单，原料来源丰富，氢化大豆油的催化活性很高，对比镍催化剂所产生的反式脂肪酸含量很低，选择性好，氢化油脂的品质好。
Description
技术领域
本发明涉及催化剂技术领域，具体涉及一种油脂氢化催化剂。
背景技术
目前氢化作为油脂深加工重要的改性过程，可以改变油脂的天然结构和甘油三酯组成。由于天然植物油中存在许多顺式不饱和脂肪酸，在光照或空气中易发生氧化、酸败，因此人们通过氢化反应将氢加到脂肪酸的不饱和双键上，使富含多不饱和脂肪酸的天然植物油转变成以单不饱和脂肪酸为主的氢化油，使得油脂的熔、沸点升高，提高油脂的氧化稳定性，延长货架期，可塑性增强，缓和油脂的臭味和风味劣化。
食用油加氢一般是以还原性镍等金属为催化剂，对油脂中存在的不饱和键催化加氢的过程，所得到的油脂称为氢化油。目前传统工业上大规模生产的氢化油主要以金属镍、铜为催化剂，由于镍系催化剂具有致癌性，而铜系催化剂会产生大量反式脂肪酸，且微量铜存在会加速油脂氧化酸败。且氢化过程的高温、高压、催化条件也会导致大量的反式脂肪酸(trans fatty acids)产生，不同氢化植物油中反式脂肪酸的含量因加工工艺的不同而有很大差异。
研究表明，TFA可以增加人们患心血管疾病和Ⅱ型糖尿病的危险性，影响儿童生长发育，增加癌症风险等。由于对健康存在危害，TFA已成为政府、学术界、食品加工业和普遍民众关注的热点问题。国内外众多研究都致力于寻求在氢化过程中减少 TFA生成量的方法。通过控制适宜的氢化操作条件(温度、压力、搅拌速度)，选择合适的贵金属催化剂、添加剂如胺类物质、无机磷酸、游离脂肪酸等，或者采用超临界流体氢化和电化学氢化反应等方法，均能减少氢化油脂中反式脂肪酸的含量。
发明内容
本发明的目的在于克服现有技术的不足，提供本发明的目的是通过以下技术方案实现的：油脂氢化催化剂：催化剂中金属铂含量为载体二氧化锆重量的1.79％，其中载体二氧化锆ZrO2的比表面积为26.3203mg，孔径为15.52589nm，金属铂分散负载在载体上，颗粒大小1±0.25nm。
本发明制备的催化剂成品的表征规格为：铂实际负载量为1.79％(以载体重量为基准)，其催化剂的比表面积(BET)为32.88mg,比孔容为0.133cmg,平均孔径为16.16nm，铂粒径大小约为1±0.25nm。根据XRD图谱显示负载的金属元素铂分别在2θ＝39.78°、2θ＝46.26°、2θ＝67.48°处发现其111面、200面与220面，说明载体表面无铂的氧化物存在，还原的充分完全。
本发明合成的催化剂的特点是：制备工艺简单，还原后活性金属稳定，原料来源丰富。与工业镍催化剂对比，本法制得的催化剂活性高，选择性好，在碘值为70-90时反式酸含量更低，氢化后油脂的品质很好：酸价稳定且小于1.0mg(KOH)/g；油脂的滑动熔点值显著上升，最终高达45.08℃。
具体实施方式
以下描述用于揭露本发明以使本领域技术人员能够实现本发明。以下描述中的优选实施例只作为举例，本领域技术人员可以想到其他显而易见的变型。
实施例1
催化剂的制备条件：
(1)载体ZrO2的制备：将硝酸氧锆固体配成水溶液，逐渐加入氨水溶液(1mol/L)直至产生沉淀物。将其离心，洗涤至中性。所的固体在110℃烘干，最后置于550℃的马弗炉中焙烤5h；
(2)称取160000μg的六水合氯铂酸固体，用蒸馏水溶解后加入3g二氧化锆载体配成2％Pt/ZrO2(载体重量为基准物)。用ICP-AES测定出铂的实际负载量为1.79％ Pt/ZrO2(载体重量为基准物)；
(3)将氯铂酸溶液与二氧化锆载体在常温下连续搅拌16h，搅拌均匀后置于旋转蒸发仪内减压蒸干；
(4)将合成的固体转移至表面皿上，于60℃真空干燥。然后置于450℃马弗炉中焙烤5h；
(5)最后将焙烧后的催化剂置于管式炉中还原活化6h，还原活化为在密闭的管式炉中通氮气吹扫以10℃/min的速率程序升温至500℃，将氮气置换成高纯氢气，在氢气流速为30mL/min的气氛中还原活化6h。制备好的催化剂使用氮气密封保存。
在本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是本发明的原理，在不脱离本发明精神和范围的前提下本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明的范围内。本发明要求的保护范围由所附的权利要求书及其等同物界定。
Claims (1)
1.一种油脂氢化催化剂，其特征在于：催化剂中金属铂含量为载体二氧化锆重量的1.79％，其中载体二氧化锆ZrO2的比表面积为26.3203mg，孔径为15.52589nm，金属铂分散负载在载体上，颗粒大小1±0.25nm。
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