CN203382745U - Complete set of production line for producing environment-friendly plasticizer - Google Patents
Complete set of production line for producing environment-friendly plasticizer Download PDFInfo
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- CN203382745U CN203382745U CN201320468421.8U CN201320468421U CN203382745U CN 203382745 U CN203382745 U CN 203382745U CN 201320468421 U CN201320468421 U CN 201320468421U CN 203382745 U CN203382745 U CN 203382745U
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Abstract
The utility model provides a complete set of production line for producing an environment-friendly plasticizer, belonging to the field of environment-friendly plasticizer preparation devices. The complete set of production line is used for preparing an environment-friendly plasticizer to replace a phthalate plasticizer, and sequentially comprises a raw material treating phase, an ester exchanging phase, an ester separation phase and an epoxidation phase which are independent to one another, wherein the raw material treating phase is used for treating plant oil raw materials; the ester exchanging phase is used for carrying out ester exchange on low-carbon alcohols under a catalytic condition to obtain glycerol; the ester separation phase is used for separating a saturated low-carbon alcohol ester from an unsaturated low-carbon alcohol ester; the epoxidation phase is used for carrying out epoxidation on an unsaturated fatty acid low-carbon alcohol ester by an epoxidation agent. The four process phases can produce corresponding products relatively and independently and can also be connected in series to carry out semi-continuous production. The complete set of production line can effectively save energy, is favorable for environmental friendliness, is moderate is investment, is simple and convenient to operate, and guarantees the quality of products; the complete set of production line is particularly suitable for preparing the environment-friendly plasticizer by palm oil, and also can be used for producing chemical intermediate byproducts.
Description
Technical field
The utility model belongs to environment-friendly plasticizer preparation facilities field, relates to a kind of complete production line of producing environment-friendly plasticizer.
Background technology:
Softening agent is auxiliary chemicals commonly used in a kind of plastics-production, and Main Function is to reduce polymer melt viscosity and melt temperature, increases polymkeric substance plasticity-and mobility, makes plastics have snappiness.Current most popular softening agent is phthalic ester plasticizer, as dibutyl phthalate (DBP), dioctyl phthalate (DOP) (DOP), diisononyl phthalate (DINP) etc.But because this type of softening agent contains phenyl ring, poisonous and difficult degraded, in production and use procedure, people's healthy and living environment in serious threat, various countries put into effect the use of this series products of legal restrictions in succession, and, this type of softening agent derives from petroleum industry, and oil belongs to Nonrenewable resources, along with rising violently and petroleum resources day by day in short supply of international oil price, therefore, invention can substitute the environment-friendly plasticizer of phthalic ester plasticizer and the inexorable trend that preparation technology has become industry thereof.Epoxy plasticiser is a kind of environment-friendly plasticizer, its chemical structure is different from phthalic ester plasticizer, it is the compound that there is epoxide group in molecular structure, and raw material comes from the animal-plant oil of self-sow, its advantage is that toxicity is minimum, heat-resisting, fast light, good stability, has been allowed for the wrapping material of food and medical treatment in many countries.
Plam oil is second-biggest-in-the-world vegetables oil, be only second to soybean oil, and its cost ratio rapeseed oil and soybean oil are low, utilize plam oil to produce environment-friendly plasticizer and there is good economic feasibility, the disclosed method prepared containing epoxyfatty acid ester of low-carbon alcohol plasticizer materials with plam oil of CN102703224A on October 3rd, 2012 discloses the method for preparing environment-friendly plasticizer with plam oil, at present, there is not yet report for the complete production line from material plant oil to the finished product environment-friendly plasticizer.
Summary of the invention
The technical problem solved:
Provide and take the complete production line that vegetables oil is the raw material production environment-friendly plasticizer, be particularly useful for take plam oil and prepare the needs of environment-friendly plasticizer as raw material, can produce the softening agent containing the epoxyfatty acid ester of low-carbon alcohol, be conducive to environmental protection, satisfy social needs, invest moderate simultaneously, easily implement, easy and simple to handle, and stage production intermediates as required, be conducive to save energy.
The technical scheme adopted:
Produce the complete production line of environment-friendly plasticizer, sequentially comprise four relatively independent operation stages, the treatment stage of raw material, transesterify stage, ester separation phase and epoxidation stage;
The treatment stage of described raw material, by the strainer with heating unit be connected in turn, the still that comes unstuck, depickling still, the first washing kettle, the first still kettle, stock oil transfer tank with heating unit, formed; The still that comes unstuck also has entrance to connect the first hot water basin, also has outlet to connect successively settling bowl and raw phospholipid basin; The depickling still also has entrance to connect the alkali lye basin, also has outlet to connect successively acidifying still and lipid acid basin, and the acidifying still also has entrance to connect the acid solution basin; The first washing kettle also has entrance to connect the second hot water basin;
The described transesterify stage is comprised of the transesterification reactor with reflux exchanger be connected in turn, the second washing kettle, after-fractionating still, fatty acid ester of low-carbon alcohol transfer tank with heating unit; The stock oil transfer tank with heating unit in the treatment stage that transesterification reactor with reflux exchanger having entrance to connect raw material also has entrance to connect the first pure basin and the first catalyzer basin simultaneously; The second washing kettle also has entrance to connect the 3rd hot water basin; Transesterification reactor with reflux exchanger also has outlet to be connected with heavy phase waste liquid recycle device;
Described ester separation phase is comprised of the crystallization kettle be connected in turn, emulsifying kettle, whizzer, the 3rd washing kettle, the 4th still kettle, unsaturated fatty acids acid low carbon alcohol ester transfer tank with heating unit; Crystallization kettle has entrance to connect the fatty acid ester of low-carbon alcohol transfer tank with heating unit in the transesterify stage; Emulsifying kettle also has entrance to connect the cold water basin; The 3rd washing kettle also has entrance to connect the 4th hot water basin; The light phase (liquid) of whizzer pumps into the 3rd washing kettle, and the heavy phase of whizzer (solid) pumps into the refining plant of saturated fatty acid low carbon alcohol ester;
The described epoxidation stage is comprised of the epoxidation reaction still with reflux exchanger be connected in turn, the 5th washing kettle, the 6th still kettle, softening agent basin; Epoxidation reaction still with reflux exchanger has entrance to connect the unsaturated fatty acids acid low carbon alcohol ester transfer tank with heating unit in the ester separation phase, also has entrance shack oxygenant basin, also has outlet to connect successively in second and still, the second salt basin; In second, with still, also have entrance to be connected the second neutralizer basin; The 5th washing kettle also has entrance to connect the 6th hot water basin.
Beneficial effect:
Produce the complete production line of environment-friendly plasticizer, be particularly useful for take hair plam oil or palm olein oil as the raw material production environment-friendly plasticizer, also can be widely used in the plurality of raw materials vegetables oil: soybean oil, Viscotrol C, rapeseed oil, peanut oil, Fructus Maydis oil, sunflower seed oil, Oleum Cocois and acidifying wet goods, the use of connecting successively of described four operation stages, can carry out the semi-continuous production of environment-friendly plasticizer, each operation stage also can independently be produced corresponding product, and can obtain corresponding by product, be conducive to produce corresponding chemical industry intermediates; Therefore also be convenient to recycle intermediate raw material, be conducive to energy-conservationly, environmental, and invest moderately, easy and simple to handle, easy to control, quality product is secure; The epoxy aliphatic acid methyl ester environment-friendly plasticizer of producing is functional, can satisfy the demand fully.
The accompanying drawing explanation
The complete production line structure composition frame chart of Fig. 1, environment-friendly plasticizer.
Embodiment
Further explanation in detail by reference to the accompanying drawings; In figure, arrow is shown the medium flowing direction.
As shown in Figure 1, the structure treatment stage of described raw material is composed as follows, by the strainer 1-1 with heating unit be connected in turn, the still 1-2 that comes unstuck, depickling still 1-3, the first washing kettle 1-4, the first still kettle 1-5, the stock oil transfer tank 1-6 with heating unit forms; The still 1-2 that comes unstuck also has entrance to connect the first hot water basin 1-21, also has outlet to connect successively settling bowl 1-22 and raw phospholipid basin 1-23; Depickling still 1-3 also has entrance to connect alkali lye basin 1-31, also has outlet to connect successively acidifying still 1-32 and lipid acid basin 1-33, and acidifying still 1-32 also has entrance to connect acid solution basin 1-34; The first washing kettle 1-4 also has entrance to connect the second hot water basin 1-41;
The described transesterify stage is comprised of the 2-1 of the transesterification reactor by reflux exchanger be connected in turn, the second washing kettle 2-2, after-fractionating still 2-3, fatty acid ester of low-carbon alcohol transfer tank 2-4 with heating unit; The stock oil transfer tank 1-6 with heating unit in the treatment stage that transesterification reactor 2-1 with reflux exchanger having entrance to connect raw material also has entrance to connect the first pure basin 2-11 and the first catalyzer basin 2-12 simultaneously; The second washing kettle 2-2 also has entrance to connect the 3rd hot water basin 2-21; It is as follows that transesterification reactor 2-1 with reflux exchanger also has outlet to be connected with heavy phase waste liquid recycle device, and transesterification reactor 2-1 also has outlet to connect successively in first and still 2-13, the 3rd still kettle 2-16 and the second pure basin 2-17; In first, with still 2-13, also have entrance to be connected the first neutralizer basin 2-14, also have outlet to connect the first salt basin 2-15; The 3rd still kettle 2-16 also has outlet to connect raw glycerine basin 2-18;
Described ester separation phase is by the crystallization kettle 3-1 be connected in turn, emulsifying kettle 3-2, whizzer 3-3, the 3rd washing kettle 3-4, the 4th still kettle 3-5, and the unsaturated fatty acids acid low carbon alcohol ester transfer tank 3-6 with heating unit forms; Crystallization kettle 3-1 has entrance to connect the fatty acid ester of low-carbon alcohol transfer tank 2-4 with heating unit in the transesterify stage; Emulsifying kettle 3-2 also has entrance to connect cold water basin 3-21; The 3rd washing kettle 3-4 also has entrance to connect the 4th hot water basin 3-41; The light phase (liquid) of whizzer 3-1 pumps into the 3rd washing kettle 3-4; The refining plant of saturated fatty acid low carbon alcohol ester is as follows, the heavy phase of whizzer 3-1 (solid) pumps into the breakdown of emulsion still 3-31 with steam bypass structure, and breakdown of emulsion still 3-31 outlet connects successively the 4th washing kettle 3-32, the 5th still kettle 3-33 and has the saturated fatty acid low carbon alcohol ester basin 3-34 of heating unit; The 4th washing kettle 3-32 also has entrance to connect the 5th hot water basin 3-35;
The described epoxidation stage is comprised of the epoxidation reaction still 4-1 with reflux exchanger, the 5th washing kettle 4-2, the 6th still kettle 4-3, the softening agent basin 4-4 that are connected in turn; Epoxidation reaction still 4-1 with reflux exchanger has entrance to connect the unsaturated fatty acids acid low carbon alcohol ester transfer tank 3-6 with heating unit in the ester separation phase, also have entrance shack oxygenant basin 4-11, also have outlet to connect successively in second and still 4-12 and the second salt basin 4-14; In second, with still 4-12, also have entrance to be connected the second neutralizer basin 4-13; The 5th washing kettle 4-2 also has entrance to connect the 6th hot water basin 4-21.
Pipeline, valve or dehvery pump are set between the equipment in described each operation stage and between each operation stage according to need to be realized interconnecting.
Described each hot water basin all can adopt the heating of steam through type, or adopts indirect heating apparatus;
Described heating unit is one or more the combination in outer clip shell type, external coiled pipe type, internal coil-tube type, and heating medium used is steam, hot water or thermal oil.
Breakdown of emulsion still 3-31 adopts the straight-through type of heating of steam.
Described each still kettle all adopts vacuum distillation apparatus, corresponding condenser, surge tank, vacuum apparatus, consists of, control the relative vacuum degree and be-0.09～-0.03MPa, temperature is 60～95 ℃.
Transesterification reactor 2-1 and epoxidation reaction still 4-1 need be equipped with take the reflux exchanger that cold water is medium.
Water temperature in cold water basin 3-21 is controlled at 10～14 ℃, with indirect cooling realization of heat-eliminating medium (cold water, refrigerating fulid).
Intermediate raw material used:
In the treatment stage of raw material, the alkali lye for saponification in alkali lye basin 1-31 is NaOH solution, and the acid solution for the invert soap compound in acid solution basin 1-34 is dilute hydrochloric acid or dilution heat of sulfuric acid;
In the transesterify stage, the monohydroxy-alcohol that is carbonatoms 1～10 for the low-carbon alcohol of transesterify in the first pure basin 2-11, catalyzer for transesterify catalysis in the first catalyzer basin 2-12 is the vitriol oil or Phenylsulfonic acid etc., and the dilute alkaline soln for neutralization in the first neutralizer basin 2-14 is NaOH or Na
2cO
3deng solution;
Epoxidation is in the stage, the hydrogen peroxide that the epoxidizing agent in epoxidizing agent basin 4-11 is concentration 30～50%, hydrogen peroxide and organic acid mixture or be the peroxide organic acid.
Dilute alkaline soln for neutralization in the second neutralizer basin 4-13 is NaOH or Na
2cO
3deng solution.
Embodiment
Take the hair plam oil as the raw material production environment-friendly plasticizer, and the hair plam oil is that palm fruit directly squeezes the plam oil obtained.
The treatment stage of A, raw material
Will be containing a solid impurity more hair plam oil is heated to 70～90 ℃ and pumps into strainer 1-1, and after filtering, filtrate the joining still 1-2 that comes unstuck, add hot water by the first hot water basin 1-21, at 70～90 ℃, slowly stirs and within 1 hour, carry out degumming process; Come unstuck and finish rear stratification, upper strata is degummed oil, and lower floor is the phospholipid colloid, and the phospholipid colloid is isolated solid impurity after settling bowl 1-22, and it is stand-by that liquid raw phospholipid deposits raw phospholipid basin 1-23 in; Degummed oil enters depickling still 1-3, add alkaline solution by alkali lye basin 1-31 in depickling still 1-3, under 50～70 ℃, general's free fatty acids saponification wherein is 1 hour, stratification afterwards, heavy phase is soap lye, pump into acidifying still 1-32, by acid solution basin 1-34, add acid solution to make saponified in soap lye be converted into lipid acid (being mainly stearic acid), and separate from water and deposit lipid acid basin 1-33 in; Depickling still 1-3 gently enters the first washing kettle 1-4 for the depickling oil pump mutually, add 50～70 ℃ of hot water by the second hot water basin 1-41, after being washed to neutrality, entering the first still kettle 1-5 carries out underpressure distillation and dewaters, must be after the depickling of coming unstuck and meet the stock oil of next stage working conditions, deposit stock oil transfer tank 1-6 in.
B, transesterify stage
Stock oil is added to transesterification reactor 2-1, add methyl alcohol by the first pure basin 2-11, add catalyzer by the first catalyzer basin 2-12, stir and carry out transesterification reaction 1 hour under 50～70 ℃, stratification after reaction finishes, lower floor is the heavy phase waste liquid, waste liquid enters in first and still 2-13, by the first neutralizer basin 2-14, add dilute alkaline soln to obtain the salt precipitation, cross the filter cake thing and deposit the first salt basin 2-15 in, non-throw out pumps into the 3rd still kettle 2-16, it is stand-by that underpressure distillation recovery methyl alcohol deposits the second pure basin 2-17 in, remaining liquid deposits raw glycerine basin 2-18 in, can further process to obtain refining glycerine, the upper strata of reactor 2-1 is that light phase crude fatty acid methyl ester pumps into the second washing kettle 2-2, add 50～70 ℃ of hot water by the 3rd hot water basin, after being washed to neutrality, entering after-fractionating still 2-3 carries out underpressure distillation and dewaters, obtain the fatty acid methyl ester of anhydrous mixing, be mainly the mixture of oleic acid (unsaturated), linolic acid (unsaturated), palmitinic acid (saturated) and stearic acid (saturated) methyl esters, deposit fatty acid ester of low-carbon alcohol transfer tank 2-4 in.
C, ester separation phase
The fatty acid methyl ester of anhydrous mixing is added to crystallization kettle 3-1, cool, when crystallization occurring, cooling should slowly be carried out, and control temperature and time, when solid content reaches 40～60% left and right, enter emulsifying kettle 3-2, add low temperature emulsified water and stir simultaneously by cold water basin 3-21 simultaneously, enter whizzer 3-3 after for some time and separate solid-liquid, light phase (liquid) pumps into the 3rd washing kettle 3-4, add 50～70 ℃ of hot water by the 4th hot water basin 3-41, after being washed to the emulsification disappearance, enter the 4th still kettle 3-5, underpressure distillation dewaters, obtain anhydrous unsaturated fatty acids methyl esters, deposit unsaturated fatty acids acid low carbon alcohol ester transfer tank 3-6 in, heavy phase in whizzer 3-3 (solid) pumps into breakdown of emulsion still 3-31, pass into water vapor and carry out breakdown of emulsion, and oil phase is pumped into to the 5th still kettle 3-33 underpressure distillation dewater, obtain anhydrous saturated fatty acid methyl ester, it is mainly palmitinic acid (palmitic acid) methyl esters, deposit saturated fatty acid low carbon alcohol ester basin 3-34 in, can further process, obtain important chemical intermediate.
D, epoxidation stage
By anhydrous unsaturated fatty acids methyl esters, mainly oleic acid, methyl linoleate, add epoxidation reaction still 4-1, add by epoxidizing agent basin 4-11 the hydrogen peroxide that concentration is 40%, stir and carry out epoxidation reaction 6-8 hour under 50～80 ℃, stratification after reaction finishes, lower floor is that the heavy phase waste liquid enters in second and still 4-12, by the second neutralizer basin 4-13, add dilute alkaline soln to obtain the salt precipitation, deposit the second salt basin 4-14 in; The upper strata of epoxidation reaction still 4-1 for gently mutually thick epoxy aliphatic acid methyl ester pump into the 5th washing kettle 4-2, add 50～70 ℃ of hot water by the 6th hot water basin 4-21, be washed to neutrality, entering the 6th still kettle 4-3 carries out underpressure distillation and dewaters, obtain anhydrous epoxy aliphatic acid methyl ester, be environment-friendly plasticizer, deposit softening agent basin 4-4 in.
Test-results shows, the present invention is feasible, and trial product one epoxyfatty acid environment protection carbinol softening agent is functional, can satisfy the demand fully.
In application, according to different plant material oil, processing condition need corresponding adjustment.
Claims (3)
1. produce the complete production line of environment-friendly plasticizer, sequentially comprise four relatively independent operation stages, the treatment stage of raw material, transesterify stage, ester separation phase and epoxidation stage;
The treatment stage of described raw material, by the strainer with heating unit be connected in turn, the still that comes unstuck, depickling still, the first washing kettle, the first still kettle, stock oil transfer tank with heating unit, formed; The still that comes unstuck also has entrance to connect the first hot water basin, also has outlet to connect successively settling bowl and raw phospholipid basin; The depickling still also has entrance to connect the alkali lye basin, also has outlet to connect successively acidifying still and lipid acid basin, and the acidifying still also has entrance to connect the acid solution basin; The first washing kettle also has entrance to connect the second hot water basin;
The described transesterify stage is comprised of the transesterification reactor with reflux exchanger be connected in turn, the second washing kettle, after-fractionating still, fatty acid ester of low-carbon alcohol transfer tank with heating unit; The stock oil transfer tank with heating unit in the treatment stage that transesterification reactor with reflux exchanger having entrance to connect raw material also has entrance to connect the first pure basin and the first catalyzer basin simultaneously; The second washing kettle also has entrance to connect the 3rd hot water basin; Transesterification reactor with reflux exchanger also has outlet to be connected with heavy phase waste liquid recycle device;
Described ester separation phase is comprised of the crystallization kettle be connected in turn, emulsifying kettle, whizzer, the 3rd washing kettle, the 4th still kettle, unsaturated fatty acids acid low carbon alcohol ester transfer tank with heating unit; Crystallization kettle has entrance to connect the fatty acid ester of low-carbon alcohol transfer tank with heating unit in the transesterify stage; Emulsifying kettle also has entrance to connect the cold water basin; The 3rd washing kettle also has entrance to connect the 4th hot water basin; The light phase (liquid) of whizzer pumps into the 3rd washing kettle, and the heavy phase of whizzer (solid) pumps into the refining plant of saturated fatty acid low carbon alcohol ester;
The described epoxidation stage is comprised of the epoxidation reaction still with reflux exchanger be connected in turn, the 5th washing kettle, the 6th still kettle, softening agent basin; Epoxidation reaction still with reflux exchanger has entrance to connect the unsaturated fatty acids acid low carbon alcohol ester transfer tank with heating unit in the ester separation phase, also has entrance shack oxygenant basin, also has outlet to connect successively in second and still, the second salt basin; In second, with still, also have entrance to be connected the second neutralizer basin; The 5th washing kettle also has entrance to connect the 6th hot water basin.
2. the complete production line of production environment-friendly plasticizer according to claim 1, it is characterized in that: described heavy phase waste liquid recycle device is as follows, and transesterification reactor (2-1) also has outlet to connect successively in first and still (2-13), the 3rd still kettle (2-16), the second pure basin (2-17); In first, with still (2-13), also have entrance to be connected the first neutralizer basin (2-14), also have outlet to connect the first salt basin (2-15); The 3rd still kettle (2-16) also has outlet to connect raw glycerine basin (2-18).
3. the complete production line of production environment-friendly plasticizer according to claim 1 and 2, it is characterized in that: the refining plant of described saturated fatty acid low carbon alcohol ester is as follows, the heavy phase (solid) of whizzer (3-1) pumps into the breakdown of emulsion still (3-31) with steam bypass structure, and breakdown of emulsion still (3-31) outlet connects successively the 4th washing kettle (3-32), the 5th still kettle (3-33) and has the saturated fatty acid low carbon alcohol ester basin (3-34) of heating unit; The 4th washing kettle (3-32) also has entrance to connect the 5th hot water basin (3-35).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107964026A (en) * | 2017-11-28 | 2018-04-27 | 江南大学 | A kind of method that environment-friendly plasticizer is prepared by epoxidation phosphatide |
-
2013
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107964026A (en) * | 2017-11-28 | 2018-04-27 | 江南大学 | A kind of method that environment-friendly plasticizer is prepared by epoxidation phosphatide |
| CN107964026B (en) * | 2017-11-28 | 2020-03-31 | 江南大学 | Method for preparing environment-friendly plasticizer through epoxidized phospholipid |
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