Process method for efficiently removing residue of plasticizer in extract

A process method and technology of plasticizer, applied in food science and other directions, can solve the problems of long production cycle, complex process flow, increase production cost, etc., and achieve the effect of high degree of automation, simple production process and improved production efficiency

Pending Publication Date: 2020-09-04
劲牌持正堂药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since ethyl acetate is partially soluble in the water phase, the ethyl acetate dissolved in the water phase after stratification remains a plasticizer. It is necessary to increase the solvent multiple or increase the number of extractions to obtain mulberry anthocyanins with qualified plasticizers. The process flow of this method Complicated, cumbersome production operations, conventional batch extraction process, long production cycle and low production efficiency
[0005] CN105503974A discloses a method for removing residual plasticizers in steviol glycoside products: the method uses a special macroporous resin to treat and remove the plasticizers by adsorbing them on the resin; Acid, alkali, sewage treatment pressure is relatively high; this process needs to use a large amount of ethanol in the production process, which increases the production cost; in addition, because the process uses macroporous resin, the products produced cannot be used for ordinary food and functional food There are also many restrictions on the application of products produced by this process for health food declaration
These two plasticizer removal processes have high requirements on production equipment, and the vacuum degree or pressure conditions in production are harsh, and their application range is also limited to a certain extent.

Method used

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  • Process method for efficiently removing residue of plasticizer in extract

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] (1) Extraction: put Epimedium (di-n-butyl phthalate (DBP) 1.14mg / kg into a 5400L multi-functional extraction tank, no other phthalate plasticizer components were detected, and the plasticizing The agent residue does not meet the requirements ((DBP should be ≤0.3mg / kg)) 200kg, add 4000L 50% ethanol to extract, the extraction temperature is 85 ℃, the extraction time is 1.5h, and the number of times of extraction is 3 times. The three extractions are combined, The extract is 11300L in total.

[0049] (2) Concentration: Concentrate the extract with a vacuum concentrator at a concentration temperature of 60° C. and a vacuum of 0.06 MPa to a Brix value of 1.9% to obtain 4 000 L of a concentrate.

[0050] (3) Separation: Disc centrifuge is used for centrifugation at a speed of (7000±500) r / min, 3900L of clear and transparent centrifuged liquid is collected, and the centrifuged residue is discharged into the sewage treatment system.

[0051] (4) Extraction: use a centrifugal e...

Embodiment 2

[0056] (1) Extraction: Add 3000L 20% ethanol (prepared with edible alcohol and purified water) in the 4000L alcohol sinking tank, drop into the Epimedium extract (icariin content is 10.7%; DBP 13.5mg / kg, no other phthalate plasticizer components were detected, and did not meet the requirements) 100kg, heated to 40-50°C and kept stirring to dissolve, stirring time 0.5h.

[0057] (2) Concentration: Concentrate the centrifuged supernatant with a vacuum concentrator at a concentration temperature of 70°C and a vacuum of 0.075MPa until the feed liquid has no obvious ethanol smell to obtain a concentrated liquid of about 2000L with a Brix value of 5.5%.

[0058] (3) Separation: A disc centrifuge is used for high-speed centrifugal separation at a rotational speed of (7000±500) r / min. A total of 1900L of clear and transparent centrifuged liquid is collected, and the centrifuged residue is discharged into the sewage treatment system.

[0059] (4) Extraction: Use a centrifugal extractor...

Embodiment 3

[0064] (1) Extraction: Put the deoiled peach kernel cake (di(2-ethyl)hexyl phthalate (DEHP) at 3.6mg / kg into a 5400L multifunctional extraction tank, and no other phthalates were detected. Diformic acid ester plasticizer component, does not meet the requirements) 400kg, add 4000L 50% ethanol for extraction, the extraction temperature is 81°C, the extraction time is 1.5h, and the extraction times is 3 times. The extracts were combined to obtain 11 500 L of extracts.

[0065] (2) Concentration: Use a double-effect concentrator to concentrate the centrifugal supernatant under reduced pressure. The concentration temperature is 55°C and the vacuum degree is 0.08MPa. In the later stage of concentration, add water to the concentrator until the feed liquid has no obvious ethanol smell, and peach kernels are obtained. The concentrate is about 4000L, and the Brix value is 3.1%.

[0066] (3) Separation: and use a disc centrifuge for high-speed centrifugation, with a speed of (5000±500) ...

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Abstract

The invention discloses a process method for efficiently removing residue of a plasticizer in an extract. The process method comprises the steps of extraction, solid-liquid separation, extraction separation, solvent recovery and concentration, wherein the plasticizer in the extract is continuously extracted and removed through a solvent, continuous production can be achieved, an organic phase obtained after extraction can be immediately reused in subsequent production after the solvent is recovered, and the problems of high solvent consumption, emulsification phenomenon and long production period caused by intermittent treatment in the traditional extraction process are solved.

Description

technical field [0001] The invention relates to the technical field of extraction and separation, in particular to a process for removing plasticizer residues in extracts. Background technique [0002] Plasticizer, also known as plasticizer, is a polymer material additive widely used in industry to enhance flexibility. There are many kinds of commercialized plasticizers, among which phthalates (PAEs) whose raw materials come from petrochemical industry are the most. Long-term exposure to PAEs in humans may cause abnormalities in the reproductive system, and even risk of teratogenicity and cancer. On June 1, 2011, the Ministry of Health listed 17 phthalates as illegally added non-edible substances. The letter of the General Office of the Ministry of Health on the notification of the maximum residues of phthalates in food and food additives (Health Office Supervision Letter [2011] No. 551) clearly stipulates that phthalic acid bis(α- The maximum residues of ethylhexyl ester...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A23L5/20
CPCA23L5/23
Inventor 李昌瑜张露明马闯李名洁陈阳陈志元孙代华
Owner 劲牌持正堂药业有限公司
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