CN109207270A - A kind of production technology of ready denier oil acid - Google Patents
A kind of production technology of ready denier oil acid Download PDFInfo
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- CN109207270A CN109207270A CN201811157935.5A CN201811157935A CN109207270A CN 109207270 A CN109207270 A CN 109207270A CN 201811157935 A CN201811157935 A CN 201811157935A CN 109207270 A CN109207270 A CN 109207270A
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- Prior art keywords
- acid
- tall oil
- ready denier
- oil
- production technology
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- 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.)
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Classifications
-
- C—CHEMISTRY; METALLURGY
- 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
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/002—Sources of fatty acids, e.g. natural glycerides, characterised by the nature, the quantities or the distribution of said acids
-
- 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)
-
- 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
- C11B3/00—Refining fats or fatty oils
- C11B3/006—Refining fats or fatty oils by extraction
-
- C—CHEMISTRY; METALLURGY
- 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
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/08—Refining
-
- 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
Abstract
The invention belongs to industrial chemicals production fields, disclose a kind of tall oil fatty acid production process, include the following steps: (1) collect pine pulping waste liquor in it is saponified, after washing using metabisulfite solution, obtain crude tall oil soap;(2) sulfuric acid is added, obtains crude tall oil after reaction;(3) crude tall oil, solvent, additive are uniformly mixed, centrifugal treating in centrifuge is added, upper layer is taken to obtain refined tall oil;(4) refined tall oil is sent to fractionating column, fractionation obtains ready denier oil acid.It is washed using sodium sulphate to saponified, water used in traditional removal of impurities process is replaced with aromatic hydrocarbon solvent, and control the additional amount of each raw material, better impurity-eliminating effect can be obtained, finally obtained ready denier oil acid has higher purity.It is simple production process of the invention, at low cost.
Description
Technical field
The present invention relates to industrial chemicals production fields, and in particular to a kind of production technology of ready denier oil acid.
Background technique
The main component of ready denier oil acid is oleic acid and linoleic acid, and wherein abietic acid content is suitable for color less than 1%
It is dimeric dibasic acid, alkyd resin, epoxy-ester, liquid soap, fatty alcohol, amide it is required that field high, that abietic acid content is low, nitrile
Desirable feedstock;Ready denier oil acid is the cheap source of 18 carbon fatty acids, can be used for synthesizing ester emulsifier and surface treatment
Agent, the cleaning agent for the good emulsifier and Esters oil raw material in Metalworking fluid, after being also directly used as intermetallic composite coating;By
This is as it can be seen that the purposes of ready denier oil acid is very extensive, and ready denier oil acid is fractionated from tall oil, about tall oil
Preparation method also there are many kinds of.
Chinese invention patent (CN1281494, the method for preparing tall oil) discloses the preparation and processing of a kind of tall oil
Method, including neutralization procedure, intermediate treatment and boiling step, with acid reactants such as carbon dioxide, carboxylic acids in neutralization procedure
Neutralize soap (can also first use carbon dioxide, again with the neutralization of the acidic materials such as carboxylic acid);Intermediate treatment is under the conditions of 60~100 DEG C
Heating soap oil 5 minutes or more, to discharge the gas in soap oil;Boiling step is the boiling together with sulfuric acid by soap oil, mixture into
Enter separation vessel, settle and separate is at two-phase, and soap oil is on top to get arriving crude tall oil.Chinese invention patent (CN1145632,
The processing of tall oil soap) a kind of method that water separation is improved in tall oil preparation process is disclosed, including it is neutralizing zone, secondary
Neutralizing zone, water segregation section, steaming stage;The soap aqueous mixtures of neutralizing zone are neutralized with carbon dioxide, then secondary with sulfuric acid implementation
It neutralizes, the separation of the wherein water phase of potassium-containing hydrogen salt and soap can be significantly improved, then carry out boiling with sulfuric acid, obtain crude tall oil.
It include plurality of impurities containing the remaining stream operated from sulfate pulping in crude tall oil obtained by the above method, such as
Relict mineral acid, alkali metal salt and soap etc., the fatty acid purity being fractionated using common tall oil is lower, needs to thick
Tall oil is refined, and impurity is removed, and fractionation can just obtain the higher ready denier oil acid of purity.
Tall oil is carried out removal of impurities to handle highly effective method being to eliminate pitch with thin film evaporator, crude tall oil enters
It is heated rapidly in thin film evaporator, individual ready denier oil acid and tall oil pitch acid fraction, heat treatment process can be obtained
Component is caused in tall oil to have occurred side reaction, and much impurity follow tall oil pitch to stay in the bottom of thin film evaporator,
And become entrained in steam in fractional distillation process, the ready denier oil acid purity caused is not high;The method for eliminating pitch simultaneously
Many raw material that hydrogen can be added to form more valuable chemical products are also eliminated, biggish loss is caused, is unfavorable for work
Industry production.
Chinese invention patent (CN103370403, the method and apparatus purified to biological source material) discloses one kind
The method purified using mixture of the multistep evaporation process to terpenes material and tall oil material, material after purification can
For producing bio-fuel etc..This method only gives the purification process of terpenes and tall oil material mixture, is unable to get
The tall oil of high-purity also can not just be fractionated to obtain the ready denier oil acid of high-purity.
Chinese invention patent (CN104981537, the biorefining of crude tall oil) discloses a kind of refining crude tall oil
Technique can remove the impurity in crude tall oil, including (1) Carvedilol oil wash: tall oil is washed with a small amount;(2) first oil
First pre-treatment step of phase (including refined tall oil and impure water phase) separation: additive, mainly citric acid is added
And ethylenediamine tetra-acetic acid, as chelating agent, to combine the water soluble metal complexes in tall oil;Pre-treatment step is heating
It is carried out under centrifugal condition.(3) from the second step of the oily phase of the aqueous phase separation second: using isolated method is decanted, being divided
From the tall oil refined.Then, refined tall oil is sent into vacuum distillation system, fractionation obtains fatty acid and resin
Acid.Then, refined tall oil is sent into system of processing, separates 170 DEG C of volatile components below, obtain " non-volatile object it is appropriate
That oil plant stream ", then be sent in thin film evaporator, it is fractionated, takes the fraction under different boiling to get ready denier oil acid is arrived
With tall oil pitch acid.This method of purification uses water, additive, and the presence of water declines refining effect, and fractional distillation process
Thin film evaporator is still used, causes to have finally obtained ready denier oil acid purity lower.
Summary of the invention
The present invention problem to be addressed is how tall oil impurity content in existing tall oil fatty acid production process is higher, with
And the technical problem that the ready denier oil acid purity that makes of fractional method is lower.
In order to solve the above technical problems, including the following steps: the invention discloses a kind of tall oil fatty acid production process
(1) saponified in collection pine pulping waste liquor, metabisulfite solution is added, washing takes upper layer, obtains thick Carvedilol
Soap;
(2) sulfuric acid is added, after reaction, stands, takes upper layer, as crude tall oil;
(3) crude tall oil, solvent, additive are uniformly mixed, centrifugal treating in centrifuge is added, upper layer is taken to be refined
Tall oil;
(4) refined tall oil is sent to fractionating column, fractionation obtains ready denier oil acid.
It selects metabisulfite solution as detergent, is because usually using sodium hydroxide and vulcanized sodium when with pine slurrying
Pressure cooking, upper layer floating object is thick Carvedilol soap after pulping waste liquor is stood, and is that crude sulphate is saponified, wherein containing a large amount of water
Point, the impurity such as lignin, sodium salt, washed with sodium sulphate, benefit is embodied in: sodium sulphate is dissolved in after water in alkalescent, can be with
The free alkali in soap lye is removed, the intensity of acidification reaction is slowed down, increases acidification reaction rate.
Further, the mass concentration of the sodium sulphate is 1%-30%, is 5%-15%, then into one further
Step ground is 10%;Sodium sulfate concentration is too low, cannot give full play to cleaning function, and excessive concentration, and can introduce new impurity.
The mass ratio of the saponified and metabisulfite solution is 1:0.1-5, preferably 1:0.5-3, most preferably 1:1, can
To reach optimal washing effect, this is because: the dosage of sodium sulphate is more, it is better to saponified dispensing laundry effect, but
It is that one side dosage can excessively introduce impurity, on the other hand waste liquid to be treated is also more;And the dosage of sodium sulphate is not
Foot, i.e., saponified and metabisulfite solution mass ratio are 1:1 hereinafter, especially in 1:0.5 or less, are washed to saponified dispersion
Effect is washed with regard to unobvious;And when being lower than 1:0.1, then it cannot achieve to saponified washing.Therefore, comprehensively consider, it is optimal
Saponified and metabisulfite solution mass ratio is 1:1.
Further, pressure when the saponified washing is normal pressure, and temperature is 40-60 DEG C.
Further, the mass ratio of the crude tall oil soap and sulfuric acid be 1:0.1-1, preferably 1:0.2-0.6, most preferably
It is incomplete to will lead to acidification this is because: the additional amount of sulfuric acid is very few for 1:0.3;Acid adding amount is excessive, easily causes acidification reaction
Excessively, while also the impurity such as free acid can be introduced.
Further, the solvent is S-100# solvent, and S-100# solvent is aromatic hydrocarbon solvent, also known as industrial naptha,
Ingredient is 1,3,5- trimethylbenzenes, is petroleum fractionating resulting product, highly volatile.The solvent is selected, is because of rosin acid and rouge
Fat acid has good dissolution characteristics wherein, and other impurities such as neutrals etc. does not dissolve in the solvent, with conventional separation of solid and liquid
Method can must refine tall oil.The features such as solvent tool also safety and environmental protection performance is good, easily recycles.
Further, the additive is oxalic acid or citric acid, and weakly acidic oxalic acid or citric acid can be used as chelating agent, with
Transition metal impurity in crude tall oil is chelated in the form of complex compound, is formed precipitating, is removed metal impurities with this.
Further, the crude tall oil, solvent, additive mass ratio be 1:0.2-3:0.01-1, preferably 1:1:
0.1。
Further, Wei≤90 DEG C temperature Kong of the centrifuge, using centrifugal treating, promoted each reaction mass it
Between mixing, can guarantee that additive comes into full contact with the impurity component in crude tall oil, conducive to the removal of impurity;Increase temperature
Degree, Wei≤90 DEG C You Xuan are conducive to the diffusion between liquid, make to contact between mixed liquor more sufficiently, impurity-eliminating effect obviously mentions
It is high.Since the density of Carvedilol oil solution is minimum, it is in the upper layer of centrifuge tube after centrifugation, takes supernatant liquor to be fractionated and removes solvent
As refined tall oil.The centrifugal process can carry out repeatedly according to the actual situation, by supernatant liquor again with solvent, additive
Deng mixing after be put into centrifuge tube repeated centrifugation process, until impurity completely removes.
Further, the pressure of the fractionating column is -0.05 to -0.1MPa, i.e., is fractionated under vacuum conditions, is collected
The fraction that boiling range is 170-400 DEG C, as ready denier oil acid.It mainly include tall oil pitch acid in tall oil after refining
And ready denier oil acid, wherein the boiling range of ready denier oil acid is 170-400 DEG C, therefore collecting boiling range is 170-400 DEG C
Fraction, main component are ready denier oil acid.
In the present invention, the removal step of crude tall oil is increased, sodium sulphate, weak acid class additive, S-100# solvent is added
Centrifugation reaction is carried out under conditions of Deng, ≤90 DEG C Bing, can make each reactant that sufficiently reaction occur, improve impurity-eliminating effect;And
And the removal step of crude tall oil does not have to water, with impurity such as solvent method removal neutrals, easy dyeing objects.It is lower with impurity content
Refined tall oil be fractionated, the purity of obtained ready denier oil acid correspondingly also can be higher, obtained tall oil fatty
Sour apparent colour is more shallow.
Compared with prior art, tall oil fatty acid production process of the invention has the advantage that
(1) removal of impurities process is increased, ensure that the purity of tall oil.
(2) it is washed using metabisulfite solution is saponified to pulping waste liquor, and optimizes the concentration and use of metabisulfite solution
Amount, obtains better washing effect, provides good basis for the impurity removal process of next step.
(3) S-100# solvent is selected, substitutes traditional water removal of impurities mode, and reasonably adjust the additional amount of additive, solvent,
So that dedoping step is more thorough, obtained tall oil purity is higher, and then obtains purer ready denier oil acid.
(4) process is simple, does not need complicated production equipment, and processing cost is low.
Specific embodiment:
Specific embodiments of the present invention are described in detail below.
Embodiment 1
A kind of production technology of ready denier oil acid, includes the following steps:
(1) under normal pressure, the pine slurrying collected under conditions of temperature is 40-45 DEG C is saponified, and quality is added thereto
The metabisulfite solution that concentration is 10% is mixed, washing, is stood, and upper layer, as crude tall oil soap is taken, wherein saponified and sulfuric acid
The mass ratio of sodium solution is 1:1;
(2) it is slowly added to the concentrated sulfuric acid that mass fraction is 95-97%, makes the mass ratio 1 of crude tall oil soap and sulfuric acid:
0.3;Acidification reaction obtains crude tall oil;
(3) controlled at 100 DEG C, the mixed liquor of crude tall oil, S-100# solvent, oxalic acid is added in centrifuge, from
Heart processing, takes upper layer, as refined tall oil, wherein mass ratio (crude tall oil: S-100# solvent: oxalic acid)=1:1:0.1;
(4) refined tall oil is sent into fractionating column, under the vacuum condition of -0.06MPa, collecting boiling range is 170~400
DEG C fraction to get arrive ready denier oil acid.It is denoted as S1.
Embodiment 2-6
Compared with Example 1, difference is only that the tall oil fatty acid production process of embodiment 2-6: Na2SO4The matter of solution
Measure concentration, (saponified/Na2SO4Solution) mass ratio, (crude tall oil soap/H2SO4Solution) mass ratio, (crude tall oil/
S-100# solvent/additive) mass ratio, the dosage of each embodiment is as shown in table 1 below.Obtained ready denier oil acid difference
It is denoted as S2-S6.
Comparative example 1
It is identical as the production technology of embodiment 1, the difference is that: Na is not used2SO4Solution is washed to saponified.
Obtained ready denier oil acid is denoted as B1.
Comparative example 2
It is identical as the production technology of embodiment 1, the difference is that: S-100# solvent is not used, and replaces with phase homogeneity
The distilled water of amount.Obtained ready denier oil acid is denoted as B2.
Comparative example 3
It is identical as the production technology of embodiment 1, the difference is that: both do not use Na2SO4Solution does not use S-100# yet
Solvent, and with the distilled water with S-100# solvent phase homogenous quantities.Obtained ready denier oil acid is denoted as B3.
The purity of ready denier oil acid obtained in above-described embodiment and comparative example is measured using chromatography, test result is such as
Shown in the following table 1.
The technological parameter and product purity of each embodiment and comparative example of table 1
By upper table 1 it is found that the purity of the product ready denier oil acid S1-S6 of embodiment 1-6 is 96% or more, and compare
Product B1-B3 purity is 90% or so in example 1-3, illustrates the refined tall oil obtained using method of the invention purity is high,
Thus the ready denier oil acid purity being fractionated is also higher.
The preparation process of product B1 does not use Na2SO4Solution washs saponified in pine pulp waste liquid, therefore,
A large amount of impurity are also retained in thick Carvedilol soap, the removal of impurities even across the later period is handled, and purity is not also obviously improved.Product B2
Preparation process in do not use S-100# solvent, and replace with the distilled water of phase homogenous quantities, purity is not also high, illustrates S-100#
The presence of solvent has significant benefit to the purification of crude tall oil.Both Na is not used in the preparation process of product B32SO4Solution,
S-100# solvent is not used, therefore final purity is minimum.
For embodiment 1, obtained product S1 has highest purity, therefore is optimum embodiment.Relative to embodiment
1, for embodiment 2, Na2SO4The concentration of solution is relatively low, is declined to saponified washing effect, and final products S2 is caused
Purity decline;For embodiment 3, Na2SO4The concentration of solution is constant, and dosage increases, and the purity of final products S3 is also
Decline is because of excessive Na2SO4Solution is that system introduces impurity again, and purity is caused to decline;For embodiment 4, acidification step
Excessive sulfuric acid is selected to reduce the purity of product S4 also since excessive sulfuric acid becomes the impurity of system in rapid;
For embodiment 5, reduce the dosage of additive oxalic acid or citric acid, therefore transition metal impurity and other soaps in system
Complexing sufficiently cannot occur with it and precipitate, become impurity, influence the purity of product S5;For embodiment 6, increase molten
The dosage of agent S-100#, although S-100# solvent highly volatile, the volatilization of solvent are also required to the regular hour, exist with
It is formed impurity in system, reduces the purity of product S6.Integrated embodiment 1-6 can be seen that detergent Na2SO4Solution
Concentration and additional amount and H2SO4Additional amount, the suitable proportion of additional amount presence of S-100# solvent and additive of solution
And range, it is more than impurity-eliminating effect decline after the range, and influence the purity of obtained ready denier oil acid.
It can be seen that in conjunction with the embodiments with comparative example, select suitable detergent and solvent very heavy to the purification of tall oil
It wants, also reflects Na2SO4Solution and S-100# solvent have synergistic effect, improve the refining effect of tall oil jointly.
The foregoing is merely presently preferred embodiments of the present invention, is not limited to invent, all in design concept of the invention
Within, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of production technology of ready denier oil acid, which comprises the steps of:
(1) saponified in collection pine pulping waste liquor, after washing using metabisulfite solution, obtain crude tall oil soap;
(2) sulfuric acid is added, obtains crude tall oil after reaction;
(3) crude tall oil, solvent, additive are uniformly mixed, centrifugal treating in centrifuge is added, upper layer is taken to obtain refining Carvedilol
Oil;
(4) refined tall oil is sent to fractionating column, fractionation obtains ready denier oil acid.
2. the production technology of ready denier oil acid as described in claim 1, it is characterised in that: the mass concentration of the sodium sulphate
For 1-30%.
3. the production technology of ready denier oil acid as described in claim 1, it is characterised in that: described saponified and sodium sulphate is molten
The mass ratio of liquid is 1:0.1-5.
4. the production technology of ready denier oil acid as described in claim 1, it is characterised in that: pressure when the saponified washing
Power is normal pressure, and temperature is 40-60 DEG C.
5. the production technology of ready denier oil acid as described in claim 1, it is characterised in that: the crude tall oil soap and sulfuric acid
Mass ratio be 1:0.1-1.
6. the production technology of ready denier oil acid as described in claim 1, it is characterised in that: the solvent is that S-100# is molten
Agent.
7. the production technology of ready denier oil acid as described in claim 1, it is characterised in that: the additive is oxalic acid or lemon
Lemon acid.
8. the production technology of ready denier oil acid as described in claim 1, it is characterised in that: the crude tall oil, adds solvent
The mass ratio for adding agent is 1:0.2-3:0.01-1.
9. the production technology of ready denier oil acid as described in claim 1, it is characterised in that: the temperature of the centrifuge controls
Wei≤90 DEG C.
10. the production technology of ready denier oil acid as described in claim 1, it is characterised in that: the pressure of the fractionating column be-
0.05 to -0.1MPa, collect the fraction that boiling range is 170-400 DEG C, as ready denier oil acid.
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Cited By (1)
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CN111646891A (en) * | 2020-07-01 | 2020-09-11 | 中山华明泰科技股份有限公司 | Preparation method and application of medicinal composite plant fatty acid calcium |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101392148A (en) * | 2008-10-27 | 2009-03-25 | 福建农林大学 | Tall oil recovery method |
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2018
- 2018-09-30 CN CN201811157935.5A patent/CN109207270A/en active Pending
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Publication number | Priority date | Publication date | Assignee | Title |
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CN101392148A (en) * | 2008-10-27 | 2009-03-25 | 福建农林大学 | Tall oil recovery method |
Non-Patent Citations (1)
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CN111646891A (en) * | 2020-07-01 | 2020-09-11 | 中山华明泰科技股份有限公司 | Preparation method and application of medicinal composite plant fatty acid calcium |
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