CN1056175C - 在妥尔油制备过程中改进水分离的方法 - Google Patents
在妥尔油制备过程中改进水分离的方法 Download PDFInfo
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- CN1056175C CN1056175C CN95192497A CN95192497A CN1056175C CN 1056175 C CN1056175 C CN 1056175C CN 95192497 A CN95192497 A CN 95192497A CN 95192497 A CN95192497 A CN 95192497A CN 1056175 C CN1056175 C CN 1056175C
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- 239000000344 soap Substances 0.000 title claims abstract description 27
- 239000003784 tall oil Substances 0.000 title abstract description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 11
- 235000011089 carbon dioxide Nutrition 0.000 claims description 12
- 230000003472 neutralizing effect Effects 0.000 claims description 8
- 238000009835 boiling Methods 0.000 claims description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- -1 hydrogen salt Chemical class 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 238000010025 steaming Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 abstract description 10
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 5
- 239000001569 carbon dioxide Substances 0.000 abstract description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 abstract 1
- 239000008346 aqueous phase Substances 0.000 abstract 1
- 238000010411 cooking Methods 0.000 abstract 1
- 238000002474 experimental method Methods 0.000 description 6
- 239000002253 acid Substances 0.000 description 3
- 230000029087 digestion Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000011122 softwood Substances 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B13/00—Recovery of fats, fatty oils or fatty acids from waste materials
- C11B13/02—Recovery of fats, fatty oils or fatty acids from waste materials from soap stock
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B13/00—Recovery of fats, fatty oils or fatty acids from waste materials
- C11B13/005—Recovery of fats, fatty oils or fatty acids from waste materials of residues of the fabrication of wood-cellulose (in particular tall-oil)
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Fats And Perfumes (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Detergent Compositions (AREA)
- Lubricants (AREA)
Abstract
本发明涉及一种在妥尔油制备过程中改进水分离的方法，所述制备过程包括皂水混合物与二氧化碳中和的中和段、含碳酸氢盐的水相与皂分离的水分离段和前段所得的皂用硫酸蒸煮形成妥尔油的蒸煮段，所述改进包括在用二氧化碳中和之后但在水分离段之前，用硫酸进行二次中和的步骤。发明还涉及包括上述各段在内的制备妥尔油的方法。
Description
本发明涉及在妥尔油制备过程中改进水分离的方法，所述制备过程包括其中妥尔油皂和水的混合物用二氧化碳中和的中和段、其中含碳酸氢盐的水相与皂分离的水分离段、以及其中前段所得的皂与硫酸蒸煮(cook)形成妥尔油的蒸煮段。
在软材的碱性消化，特别是在硫酸盐法(sulfate process)中，形成通常所说的黑液，其中含有下文称为粗皂的粗妥尔油皂。这种粗皂可以用硫酸分解形成粗妥尔油。
在本说明书开始时述及的那类以二氧化碳中和作用为基础的妥尔油制备方法在USP.3,901,869中已知。此已知方法的第一阶段是实施二氧化碳的中和作用。在此阶段后，实现水的分离并在最后用硫酸蒸煮妥尔油。
粗皂用二氧化碳处理时，二氧化碳溶于皂-水乳液中，所形成的碳酸中和皂和与之伴生的碱液。中和作用将皂-水混合物的pH值降低至7.5-8.0范围。
就无机相和有机相的分离而言，最好将pH值降低0.5-1.0单位，但不使用过量的二氧化碳，因为这样将导致起泡。二氧化碳使用的最高效率是方法经济性的一个关键因素。
目前工艺水平的技术中存在的问题是水的分离不良。水的不良分离导致下一步蒸煮过程中消耗过多的硫酸，并且过量的水不必要地扩大方法的周期。过量含CO2的水在与硫酸蒸煮时还会因蒸煮过程中碳酸氢盐的分解而引起起泡。
本发明的目的是在妥尔油制备过程中改进水分离的方法。
按照本发明，在妥尔油制备过程中改进水分离的方法，包括：
其中皂水混合物用二氧化碳中和的中和段；
其中含碳酸氢盐的水相与皂分离的水分离段，和
其中前段所得的皂与硫酸蒸煮形成妥尔油的蒸煮段；
其特征在于，在用二氧化碳中和之后但在水分离段之前，用硫酸进行二次中和，在用硫酸中和后pH值达到7.2-7.6。
本发明基于这样的认识，即在用二氧化碳中和后，加入硫酸实施二次中和时，可显著地改进在水分段中水的分离。随着加入硫酸，pH值降低大约0.5-1pH单位，达到大约7.2-7.6的最佳pH值范围。硫酸的加入根据pH值而定。
在一个未加压反应器中加入硫酸，该反应器设置在二氧化碳中和反应器之后的位置，而在分离槽之前。
CO2中和反应可在常压或过压下实施。所用二氧化碳最好是气态二氧化碳。
下面参照附图对本发明进行更详细的描述，附图是本发明的妥尔油制备方法的框图。
将粗皂和水泵入CO2中和反应器，其中通入气态CO2以中和混合物。把皂和水的混合物送入H2SO4中和反应器中，向其中加入硫酸以进一步中和皂和水的混合物。随后将皂送入分离槽，在其中碳酸氢盐盐水与皂分离。最后，将皂送入妥尔油蒸煮器中进行用硫酸的酸化，此后得到粗妥尔油。
实施例
实验在一个2升的高压釜中进行。制备含500g皂和800g水的物料。仔细混合物料，然后将其转入高压釜中。皂-水混合物的初始pH值为12。将物料加热至50℃。达到温度时向高压釜中通入CO2气流，借此把釜内压力调节至11bar。高压釜阶段(120分钟)后，从物料中取出约500g样品。将样品分成二份等分试样，向其中一份试样中加入一定量的硫酸降低pH值(至7.2)并改进水的分离(根据本发明的实验A)，另一份试样中不加入硫酸(对照实验B)。然后，将混合物倒入分液漏斗中将水从各皂和碳酸氢盐盐水混合物中分出。
分析所得含水相的Na浓度(％)和CO2总量(％)。通过这些数据计算水中的NaHCO3浓度(％)。
最后用硫酸进行妥尔油蒸煮。分析得到的妥尔油的H2O和树脂酸的百分含量。
表1
实验A和B的实验结果，其中B为对照实验而A为本发明的实验。
| B | A | |
| 分离后的含水相(g) | 89 | 130 |
| 分离后的皂相(g) | 163 | 120 |
| 含水相： | ||
| Na(％) | 1.3 | 1.2 |
| CO2(％) | 1.8 | 1.4 |
| NaHCO3(％) | 1.53 | 0.95 |
| 妥尔油： | ||
| H2O(％) | 6.1 | 5.5 |
| 树脂酸(％) | 42.5 | 33.6 |
表1的结果表明，按照本发明加入硫酸可显著改进水的分离。从表1的结果可看出，补充酸化过程除去了水，并随之一起除去碳酸氢钠。从妥尔油蒸煮过程后所得妥尔油中的树脂酸含量也可得到相同的结论。通过滴定测定酸度，从结果看出，在此情况下妥尔油中的残留碳酸氢盐增加了酸度。
Claims (3)
1、一种在妥尔油制备过程中改进水分离的方法，所述制备过程包括：
其中皂水混合物用二氧化碳中和的中和段；
其中含碳酸氢盐的水相与皂分离的水分离段，和
其中前段所得的皂与硫酸蒸煮形成妥尔油的蒸煮段；
其特征在于，在用二氧化碳中和之后但在水分离段之前，用硫酸进行二次中和，在用硫酸中和后pH值达到7.2-7.6。
2、根据权利要求1的方法，其特征在于硫酸的中和作用使pH值降低0.5-1pH单位。
3、根据权利要求1或2的方法，其特征在于在常压下进行硫酸的中和作用。
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FI940969A FI95595C (fi) | 1994-03-01 | 1994-03-01 | Menetelmä vedenerottuvuuden parantamiseksi mäntyöljyn valmistusprosessissa sekä menetelmä mäntyöljyn valmistamiseksi |
| FI940969 | 1994-03-01 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1145632A CN1145632A (zh) | 1997-03-19 |
| CN1056175C true CN1056175C (zh) | 2000-09-06 |
Family
ID=8540227
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN95192497A Expired - Fee Related CN1056175C (zh) | 1994-03-01 | 1995-02-28 | 在妥尔油制备过程中改进水分离的方法 |
Country Status (12)
| Country | Link |
|---|---|
| US (1) | US5891990A (zh) |
| EP (1) | EP0748366B1 (zh) |
| JP (1) | JPH09509693A (zh) |
| CN (1) | CN1056175C (zh) |
| AT (1) | ATE176276T1 (zh) |
| AU (1) | AU1813495A (zh) |
| BR (1) | BR9506913A (zh) |
| CA (1) | CA2184244C (zh) |
| DE (1) | DE69507600T2 (zh) |
| ES (1) | ES2128714T3 (zh) |
| FI (1) | FI95595C (zh) |
| WO (1) | WO1995023837A1 (zh) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FI952176A (fi) * | 1995-05-05 | 1996-11-06 | Polargas Ab Oy | Suovan neutralointi |
| FI104491B (sv) | 1996-12-30 | 2000-02-15 | Aga Ab | Förfarande och anordning för rening av rå talloljesåpa |
| FI105569B (fi) * | 1997-12-11 | 2000-09-15 | Polargas Ab Oy | Menetelmä mäntyöljyn valmistamiseksi |
| FI110951B (fi) * | 2001-09-20 | 2003-04-30 | Valtion Teknillinen | Menetelmä suovan hapottamiseksi |
| EP1302529A1 (en) * | 2001-10-09 | 2003-04-16 | Linde AG | Brine separation in tall soap oil preparation |
| EP1637582B1 (en) * | 2004-09-21 | 2007-05-16 | Linde AG | A process for recovering tall oil or tall oil fuel |
| EP1870445A1 (en) * | 2006-06-21 | 2007-12-26 | Linde Aktiengesellschaft | Process for producing tall oil and use of heating in the production of tall oil |
| FI121427B (fi) * | 2008-06-17 | 2010-11-15 | Linde Ag | Menetelmä mäntyöljyn valmistamiseksi ja suolaliuoksen deaktivoinnin käyttö mäntyöljyn valmistuksessa |
| FI20096366A (fi) | 2009-12-18 | 2011-06-19 | Linde Ag | Menetelmä ja laite mäntyöljysuovan neutraloimiseksi |
| CN111334370A (zh) * | 2020-03-13 | 2020-06-26 | 福建省沙县松川化工有限公司 | 一种妥尔油的生产设备及其生产工艺 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3901869A (en) * | 1974-01-11 | 1975-08-26 | Westvaco Corp | Acidification of tall oil soap |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE98166C1 (zh) * |
-
1994
- 1994-03-01 FI FI940969A patent/FI95595C/fi not_active IP Right Cessation
-
1995
- 1995-02-28 US US08/702,493 patent/US5891990A/en not_active Expired - Lifetime
- 1995-02-28 ES ES95909804T patent/ES2128714T3/es not_active Expired - Lifetime
- 1995-02-28 CN CN95192497A patent/CN1056175C/zh not_active Expired - Fee Related
- 1995-02-28 BR BR9506913A patent/BR9506913A/pt not_active IP Right Cessation
- 1995-02-28 AT AT95909804T patent/ATE176276T1/de active
- 1995-02-28 AU AU18134/95A patent/AU1813495A/en not_active Abandoned
- 1995-02-28 DE DE69507600T patent/DE69507600T2/de not_active Expired - Lifetime
- 1995-02-28 JP JP52271795A patent/JPH09509693A/ja not_active Ceased
- 1995-02-28 EP EP95909804A patent/EP0748366B1/en not_active Expired - Lifetime
- 1995-02-28 CA CA 2184244 patent/CA2184244C/en not_active Expired - Fee Related
- 1995-02-28 WO PCT/FI1995/000107 patent/WO1995023837A1/en active IP Right Grant
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3901869A (en) * | 1974-01-11 | 1975-08-26 | Westvaco Corp | Acidification of tall oil soap |
Also Published As
| Publication number | Publication date |
|---|---|
| WO1995023837A1 (en) | 1995-09-08 |
| US5891990A (en) | 1999-04-06 |
| JPH09509693A (ja) | 1997-09-30 |
| AU1813495A (en) | 1995-09-18 |
| BR9506913A (pt) | 1997-09-16 |
| ATE176276T1 (de) | 1999-02-15 |
| FI95595B (fi) | 1995-11-15 |
| FI95595C (fi) | 1998-12-01 |
| FI940969A0 (fi) | 1994-03-01 |
| DE69507600T2 (de) | 1999-06-24 |
| EP0748366A1 (en) | 1996-12-18 |
| CN1145632A (zh) | 1997-03-19 |
| CA2184244C (en) | 2005-04-26 |
| ES2128714T3 (es) | 1999-05-16 |
| EP0748366B1 (en) | 1999-01-27 |
| CA2184244A1 (en) | 1995-09-08 |
| FI940969A (fi) | 1995-09-02 |
| DE69507600D1 (de) | 1999-03-11 |
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