CN116637587A - 一种啤酒硅胶及其制备方法 - Google Patents
一种啤酒硅胶及其制备方法 Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 235000013405 beer Nutrition 0.000 title claims abstract description 54
- 239000000741 silica gel Substances 0.000 title claims abstract description 52
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000003607 modifier Substances 0.000 claims abstract description 39
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000011148 porous material Substances 0.000 claims abstract description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052742 iron Inorganic materials 0.000 claims abstract description 7
- -1 iron ion Chemical class 0.000 claims abstract description 6
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
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- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
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- 229910052911 sodium silicate Inorganic materials 0.000 claims description 5
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- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 3
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 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 description 3
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 3
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
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Classifications
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28061—Surface area, e.g. B.E.T specific surface area being in the range 100-500 m2/g
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28064—Surface area, e.g. B.E.T specific surface area being in the range 500-1000 m2/g
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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
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- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
- B01J20/28073—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being in the range 0.5-1.0 ml/g
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
- B01J20/28076—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being more than 1.0 ml/g
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/28083—Pore diameter being in the range 2-50 nm, i.e. mesopores
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- Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)
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Abstract
本发明公开了一种啤酒硅胶及其制备方法。一种啤酒硅胶,其比表面积为400‑700m2/g,孔体积为0.7‑1.8ml/g,平均孔径为5‑18nm,铁离子含量小于30ppm。在硫酸溶液中加入酸类改性剂A,使Si02分子凝聚得更加牢固,使啤酒硅胶的吸附能力提高两倍以上;改性剂B改善了硅胶产品的物理性质,此种孔结构的硅胶更适用于啤酒稳定化处理,既减少了铁离子对啤酒口味的影响,使得啤酒硅胶的纯度提高,又提高了其吸附能力。该啤酒硅胶相对于传统的啤酒硅胶更容易分散,可以缩短在生产中的搅拌时间,减少空气对啤酒的影响。提高生产效率。此种啤酒硅胶选择性更好,工作范围更广。本发明的制备方法解决了普通啤酒硅胶孔径范围过宽,选择性差的问题。
Description
技术领域
本发明涉及特殊硅胶制备技术领域,尤其涉及一种低金属含量、高比表面积的,用于啤酒稳定化处理的一种啤酒硅胶及其制备方法。
背景技术
啤酒是由大麦芽发酵精制而成,其中含有大量的维生素、氨基酸、蛋白质、糖类等营养成份。在啤酒生产的过程中,会产生蛋白质大分子和多酚类物质,使啤酒产生混浊,影响了啤酒的外观及质量,进而影响啤酒的价值。因此,为了防止啤酒发生混浊,必须减少啤酒中这些引起产生混浊的组分。
目前,常采用浑浊抑制剂(稳定化处理剂)来降低啤酒中产生混浊的组分,如木瓜蛋白醇、单宁酸、PVPP(聚乙烯基聚吡咯烷酮)、甲醛和硅胶等物质。硅胶之被广泛应用,是由于硅胶是一种多微孔结构的非晶态固体粉末,主要成分为mSiO2·nH2O,除苛性钠和氢氟酸外,不溶于水和任何溶剂,不与任何酸、碱、盐反应,具有化学性质稳定的优点,并且无毒、无味、不燃,具有较强的稳定性,这样优秀的理化性质决定了硅胶完全可以作为一种有效的吸附剂来代替啤酒生产中的硅藻土等填料。
发明内容
基于上述背景技术,本发明提供一种啤酒硅胶及其制备方法。
一种啤酒硅胶,其比表面积为400-700m2/g,孔体积为0.7-1.8ml/g,平均孔径为5-18nm,铁离子含量小于30ppm。
一种啤酒硅胶的制备方法,包括以下步骤:
(1)制胶:将质量比浓度为20%-45%的硫酸溶液,加入改性剂A和质量比浓度为15%-35%的泡花碱溶液通过反应器制备得到硅胶;改性剂A为由硫酸、盐酸、硝酸、草酸、醋酸、柠檬酸、磷酸、EDTA中的一种或多种组成的混合物,所述改性剂A溶液的质量比浓度为0.1%-7.0%;
(2)清洗处理:将步骤(1)制得的产品在30℃-90℃下进行水洗处理,至湿胶显中性;
(3)改性剂B处理:将步骤(2)制得的产品在30℃-90℃下用改性剂B浸泡1-10小时,所述改性剂B为由硫酸镁、硝酸镁、氯化镁、氯化钠、硫酸铝、硝酸铝、氯化铝、碳酸氢铵、氨水中的一种或多种组成的混合物,所述改性剂B溶液的质量比浓度为0.001%-3.0%;
(4)烘干:将步骤(4)制得的产品在100℃-400℃下进行烘干后粉碎得到最终产品。
进一步的,所述改性剂A优选浓度为0.3%-6.0%。
进一步的,所述水洗处理的优选温度为40℃-70℃。
进一步的,所述改性剂B溶液浓度优选为0.07%-2.0%。
综上所述,本发明具有以下有益效果:
本发明的特点是先在硫酸溶液中加入改性剂A,再在反应器中反应缩聚,生成凝胶颗粒,又经老化、水洗,而后加入改性剂B,而后干燥的工艺处理得到的啤酒硅胶产品。由于在硫酸溶液中加入酸类改性剂A,使Si02分子凝聚得更加牢固,使啤酒硅胶的吸附能力提高两倍以上;改性剂B改善了硅胶产品的物理性质,此种孔结构的硅胶更适用于啤酒稳定化处理,既减少了铁离子对啤酒口味的影响,使得啤酒硅胶的纯度提高,又提高了其吸附能力。该啤酒硅胶相对于传统的啤酒硅胶更容易分散,可以缩短在生产中的搅拌时间,减少空气对啤酒的影响。提高生产效率。此种啤酒硅胶选择性更好,工作范围更广。本发明的制备方法解决了普通啤酒硅胶孔径范围过宽,选择性差的问题。
具体实施方式
一种啤酒硅胶,其比表面积为400-700m2/g,孔体积为0.7-1.8ml/g,平均孔径为5-18nm,铁离子含量小于30ppm。
一种啤酒硅胶的制备方法,包括以下步骤:
(1)制胶:将质量比浓度为20%-45%的硫酸溶液,加入改性剂A和质量比浓度为15%-35%的泡花碱溶液通过反应器制备得到硅胶;改性剂A为由硫酸、盐酸、硝酸、草酸、醋酸、柠檬酸、磷酸、EDTA中的一种或多种组成的混合物,所述改性剂A溶液的质量比浓度为0.1%-7.0%,所述改性剂A优选浓度为0.3%-6.0%;
(2)清洗处理:将步骤(1)制得的产品在30℃-90℃下进行水洗处理,至湿胶显中性,所述水洗处理的优选温度为40℃-70℃;
(3)改性剂B处理:将步骤(2)制得的产品在30℃-90℃下用改性剂B浸泡1-10小时,所述改性剂B为由硫酸镁、硝酸镁、氯化镁、氯化钠、硫酸铝、硝酸铝、氯化铝、碳酸氢铵、氨水中的一种或多种组成的混合物,所述改性剂B溶液的质量比浓度为0.001%-3.0%,所述改性剂B溶液浓度优选为0.07%-2.0;
(4)烘干:将步骤(4)制得的产品在100℃-400℃下进行烘干后粉碎得到最终产品。
为使本发明实施例的目的、技术方案和优点更加清楚,下面将结合本发明的实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例一
本发明的啤酒硅胶的制造方法是在20%硫酸溶液中加入改性剂A浓度1%,改性剂A添加量为硫酸量的1%,从而制成含有改性剂A的硫酸溶液。
采用常规反应器,加入浓度30%的泡花碱溶液,在45-60℃温度下反应6-9分钟,生成硅酸凝胶,又经45-60℃老化2小时,60℃水水洗,最后用0.6%改性剂B氯化镁溶液浸泡3-5小时,放掉酸溶液,用70℃的水清洗3-5遍,至胶体中的PH值7.0左右。放水后捞胶,400℃热风干燥1小时左右,从而得到平均孔径5-18mm的铁含量小于30ppm的啤酒硅胶产品。
啤酒硅胶产品指标如表1所示。
表1:啤酒硅胶的各项指标。
实施例二
本发明的啤酒硅胶的制造方法,具体为将浓度30%的硫酸与浓度17.5%的泡花碱溶液,改性剂A的浓度1.5%,用量为硫酸量的3%,经反应器混合反应后得到的硅胶放入水洗罐中,又经40-50℃老化3小时,以浓度为1.0%的改性剂B硝酸镁在65℃下,浸泡3小时。放掉酸溶液,加入50℃的水,4小时后放掉水,再加入50℃的水,如此循环操作至胶体中的PH值7.0左右。放掉水后,捞出硅胶在300℃下烘干,得到啤酒硅胶产品,指标如表2。
表2:啤酒硅胶的各项指标。
以上实施例仅用以说明本发明的技术方案,而非对其进行限制;尽管参照前述实施例对本发明进行了详细的说明,对于本领域的普通技术人员来说,依然可以对前述实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换;而这些修改或替换,并不使相应技术方案的本质脱离本发明所要求保护的技术方案的精神和范围。
Claims (5)
1.一种啤酒硅胶,其特征在于,所述啤酒硅胶的比表面积为400-700m2/g,孔体积为0.7-1.8ml/g,平均孔径为5-18nm,铁离子含量小于30ppm。
2.一种啤酒硅胶的制备方法,其特征在于,包括以下步骤:
(1)制胶:将质量比浓度为20%-45%的硫酸溶液,加入改性剂A和质量比浓度为15%-35%的泡花碱溶液通过反应器制备得到硅胶;改性剂A为由硫酸、盐酸、硝酸、草酸、醋酸、柠檬酸、磷酸、EDTA中的一种或多种组成的混合物,所述改性剂A溶液的质量比浓度为0.1%-7.0%;
(2)清洗处理:将步骤(1)制得的产品在30℃-90℃下进行水洗处理,至湿胶显中性;
(3)改性剂B处理:将步骤(2)制得的产品在30℃-90℃下用改性剂B浸泡1-10小时,所述改性剂B为由硫酸镁、硝酸镁、氯化镁、氯化钠、硫酸铝、硝酸铝、氯化铝、碳酸氢铵、氨水中的一种或多种组成的混合物,所述改性剂B溶液的质量比浓度为0.001%-3.0%;
(4)烘干:将步骤(4)制得的产品在100℃-400℃下进行烘干后粉碎得到最终产品。
3.根据权利要求2所述的一种啤酒硅胶的制备方法,其特征在于,所述改性剂A优选浓度为0.3%-6.0%。
4.根据权利要求2所述的一种啤酒硅胶的制备方法,其特征在于,所述水洗处理的优选温度为40℃-70℃。
5.根据权利要求2所述的一种啤酒硅胶的制备方法,其特征在于,所述改性剂B溶液浓度优选为0.07%-2.0%。
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