CN103044603A - Food packaging latex as well as preparation method and application thereof - Google Patents
Food packaging latex as well as preparation method and application thereof Download PDFInfo
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- CN103044603A CN103044603A CN2012105723031A CN201210572303A CN103044603A CN 103044603 A CN103044603 A CN 103044603A CN 2012105723031 A CN2012105723031 A CN 2012105723031A CN 201210572303 A CN201210572303 A CN 201210572303A CN 103044603 A CN103044603 A CN 103044603A
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Abstract
The invention discloses food packaging latex, as well as a preparation method and an application thereof. The food packaging latex is prepared by taking a certain amount of vinylidene chloride, acrylic acid-2-phthalic acid ester, vinyl cyanide and methylacrylic acid as mixed monomers, selecting specific seed emulsifier and mixed emulsifier, and adopting a specific seed emulsion polymerization method. The food packaging latex can be directly applied onto a basic material of a food packaging film, and a primer does not need to be applied, so that the production cost of food packages is greatly saved. The food packaging film coated with the food packaging latex is high in barrier property, oil-resistant, corrosion-resistant, odor-resistant, moisture-proof and mould-proof, can be directly contacted with food, and is flame-resistant and low in monomer residue content; and the food packaging latex is excellent in stability.
Description
Affiliated technical field
The present invention relates to a kind of latex, especially used for packing foods latex and its preparation method and application belongs to the novel high polymer material field.
Background technology
Polyvinylidene dichloride (PVDC) is a kind of nonpoisonous and tasteless, safe and reliable high barrier material, polyvinylidene dichloride (PVDC) latex is widely used in food product pack, except the general property with plastics, also have oil-proofness, erosion resistance, guarantor's flavor property and excellent protection against the tide, mildew-resistant, can be directly and the performances such as food contacts, also have simultaneously good printing performance.
Patent CN1535814A discloses a kind of PVDC lamination complex fire resistant cooking food packing film, the copolymer film of middle layer PVDC(vinylidene chloride and vinylchlorid) links to each other with the two-layer of both sides by the solvent-free caking agent of two component polyurethane type respectively, mainly solve high-barrier, transparent type, the resistant to elevated temperatures problem of food packaging film.Patent CN101306743A discloses a kind of milk packaging film, outer membrane is polyvinylidene chloride film, tackiness agent is wherein a kind of in single, double part polyurethane type solvent or the adhesive for solvent-free use, inboard film is the black and white polyethylene film, mainly solves the problems such as material easily absorbs water, barrier is low.
Above-mentioned packaging material for food of the prior art is multi-layer compound structure, between coating layer and basic unit binder layer need be set, and to guarantee that the packaging film that makes is indeformable, not ftracture, has complex manufacturing, equipment requirements height, the problems such as product price height.Prior art does not all propose a kind of used for packing foods latex, when coat foods packing base material, only need be coated with this latex, can make food product pack have high barrier, oil-proofness, erosion resistance, guarantor's flavor property, protection against the tide, mildew-resistant, can be directly and the performances such as food contacts.During latex coat foods packing of the present invention, need not to be coated with primer, greatly reduce the food product pack production cost, and the problem of environmental pollution of avoiding existing urethane primer to bring; Latex of the present invention has good stability simultaneously, and long storage is breakdown of emulsion not, and glue spread is little, easily coating, and level of residual monomers is low, makes the advantages such as simple.
Summary of the invention
For the above technical problem that exists in the prior art, the invention provides a kind of used for packing foods latex on the polypropylene film and its preparation method and application of coating, its good stability, long storage be breakdown of emulsion, little, the easy coating of glue spread not, alternative original solvent borne polyurethane primer, security is good, environmental protection, can directly coat on the film substrate, need not to be coated with primer, greatly save the food product pack production cost; The preparation method is simple for this latex, and working condition is controlled; By the food product packing film of its coating, have high barrier, oil-proofness, erosion resistance, guarantor's flavor property, protection against the tide, mildew-resistant, can directly contact with food, the performance such as fire-retardant.
The present invention is achieved by the following technical solutions: used for packing foods latex, formed by the emulsion polymerization way copolymerization by following reaction raw materials, and reaction raw materials and weight part are:
(1) monomer mixture is 50 parts, and described monomer mixture comprises the vinylidene chloride, the ethyl acrylate that accounts for mix monomer gross weight 4-6% that account for mix monomer gross weight 89-91%, account for the vinyl cyanide of mix monomer gross weight 0.3-0.7% and account for the methacrylic acid of mix monomer gross weight 4-6%;
(2) initiator, described initiator comprises: organo-peroxide 0.04-0.12 part and sodium formaldehyde sulphoxylate 0.04-0.12 part;
(3) seeding polymerization emulsifying agent, described seeding polymerization emulsifying agent comprise any one 0.06 part of being selected from the sodium sulfonate compounds and MA-80(chemistry sulfo-succinic acid methyl-isobutyl methyl esters salt by name, or are called Succinic Acid dihexyl sodium sulfonate) 0.14 part;
(4) blending emulsifiers, described blending emulsifiers comprises COPS-1(chemistry 2-allyl ethers by name-3-hydroxy propane-1-sodium sulfonate) 0.6 part and 2A-1 emulsifying agent (chemistry alkyl diphenyl ether disulfonate by name, commodity are called DOWFAX8390, or are DOWFAX30599) 0.5 part;
(5) auxiliary agent, described auxiliary agent comprise 0.0005 part of 0.012 part of ammonium acetate and iron protochloride.
Preferably, organo-peroxide is tertbutyl peroxide in the described initiator; The sodium sulfonate compounds is Sodium dodecylbenzene sulfonate in the described seeding polymerization emulsifying agent.
The present invention also provides the preparation method of described used for packing foods latex, adopts the preparation of seeding polymerization method, and concrete preparation process comprises:
(1) mix monomer preparation: described vinylidene chloride, ethyl acrylate, vinyl cyanide are mixed the rear 2h of stirring, for subsequent use;
(2) blending emulsifiers preparation: after described COPS-1,2A-1 emulsifying agent, methacrylic acid mixed, thin up to 10 part, the high-speed stirring mixing, for subsequent use;
(3) initiator preparation: described two kinds of initiators are diluted to respectively mass percentage concentration are 2%, for subsequent use;
(4) Seeded polymerization: deionized water or 32 parts of soft water, described auxiliary agent, described seeding polymerization emulsifying agent are added in the reactor, the envelope still is used nitrogen replacement 3 times, vacuumizes, suction accounts for the mix monomer of the mix monomer gross weight 5% that step 1 prepares, cold dispersion 0.5h is warming up to 47 ℃, is continuously pumped into the initiator for preparing with the speed of 8kg/48h, the control temperature of reaction is 55 ℃, when Pressure Drop during to 0.01-0.03MPa, seeding polymerization finishes, and obtains seed latex;
(5) letex polymerization: the speed that adds with 16h is continuously pumped into the remaining mix monomer that blending emulsifiers, step 1 that step 2 prepares make, when Pressure Drop to 0～-during 0.01MPa, reaction finishes, and adds microcrystalline wax, vacuumize, bottom valve is not opened desorption 1h, and temperature rises to 70 ℃ and keeps 1h, and bottom valve is crack, desorption 2h, then the water vapor that adds 0.1MPa filters, and obtains copolymer emulsion.
The present invention also provides the application of described used for packing foods latex in the coating food packaging film.
The present invention also provides the food product packing film that applies described used for packing foods latex.
Emulsion of the present invention has added reactive emulsifier in blending emulsifiers, improved the stability of emulsion; Further, vinylformic acid together added in letex polymerization stage and reactive emulsifier in the monomer methyl, because vinylformic acid good water solubility, its parcel to emulsifying agent is good, the polymkeric substance particle diameter that makes is evenly distributed, good emulsion stability can reach and deposit 2 years not effects of breakdown of emulsion, nothing precipitation under the normal temperature.In addition, the emulsion tackiness that makes is good, can be in the situation that is not coated with primer, directly coat on the film substrate such as food product packing film, and replace existing urethane primer.
Among the preparation method of the present invention, adopted specific feed time and process control parameter, added the auxiliary agent ammonium acetate, so that the emulsion of preparation has satisfactory stability; Further, before vacuum desorption step, add microcrystalline wax, can play the froth breaking effect, improve vacuum desorption effect, thereby reduce level of residual monomers, and microcrystalline wax is solid-state after the cooling, can recycle by filtration.
The present invention can make solid content and be about 50% copolymer latex, can coat on the polypropylene film, is used for food product pack.This latex stability is good, not breakdown of emulsion, little, the easy coating of glue spread of long storage, and security is good, environmental protection, greatly saves the food product pack production cost; The preparation method is simple for this latex, and working condition is controlled; By the food product packing film of its coating, have high barrier, oil-proofness, erosion resistance, guarantor's flavor property, protection against the tide, mildew-resistant, can directly contact with food, the performance such as fire-retardant.
The emulsion that makes can be measured with following methods:
| The mensuration project | Testing method |
| Solid content, % | GB1725-79 |
| Surface tension, mN/m | GB1725-79 |
| Viscosity, mPas | U.S. BROOKFIELD viscometer |
| The pH value | The accurate pH meter of PHS-3C |
| Density, g/cm 3 |
Latex glue spread of the present invention is measured steam penetrating capacity≤6g/ ㎡ 24h for singly being coated with 3.2g/ ㎡ according to standard GB/T 1037 condition B by the BOPP food product packing film of its coating; Measure oxygen transit dose≤18g/ ㎡ 24h according to standard GB/T19789-2005 voltameter detection method; Measure vinylidene chloride monomer residual quantity≤1mg/kg or do not detect according to standard GB/T 5009.122-2003.
Description of drawings
Fig. 1 is technological process block-diagram of the present invention.
Embodiment
Embodiment 1
(1) mix monomer preparation: vinylidene chloride 89kg, ethyl acrylate 4.5kg, vinyl cyanide 0.5kg are mixed the rear 2h of stirring, for subsequent use;
(2) mixed polymerization emulsifying agent preparation: be after 1.2kg, 2A-1 emulsifying agent 1kg, methacrylic acid 6kg mix with COPS-1, thin up is to 20kg, and the high-speed stirring mixing is for subsequent use;
(3) initiator preparation: tertbutyl peroxide 80g, sodium formaldehyde sulphoxylate 80g are diluted to respectively mass percentage concentration are 2%, for subsequent use;
(4) Seeded polymerization: be that 280g adds in the 200L reactor with deionized water or soft water 64kg, auxiliary agent ammonium acetate 20g, iron protochloride 1g, seeding polymerization emulsifying agent Sodium dodecylbenzene sulfonate 120g, MA-80, the envelope still, with nitrogen replacement 3 times, vacuumize, suction 5%(weight) mix monomer that step 1 makes, cold dispersion 0.5h, be warming up to 47 ℃, speed with 8kg/48h is continuously pumped into the initiator for preparing, the control temperature of reaction is 55 ℃, when Pressure Drop during to 0.01-0.03MPa, seeding polymerization finishes, and obtains seed latex;
(5) letex polymerization: the speed that adds with 16h is continuously pumped into the remaining mix monomer that blending emulsifiers, step 1 that step 2 prepares make, when Pressure Drop to 0～-during 0.01MPa, reaction finishes, and adds microcrystalline wax 100g, vacuumize, bottom valve is not opened desorption 1h, and temperature rises to 70 ℃ and keeps 1h, and bottom valve is crack, desorption 2h, then the water vapor that adds 0.1MPa filters, and obtains copolymer emulsion.
The emulsion parameter that makes is as follows:
Solid content (%): 50
Surface tension (mN/m): 40
Viscosity (mPas): 10
PH value: 1.5
Density (g/cm
3): 1.23
Singly be coated with emulsion that 3.2g/ ㎡ makes to the BOPP film, measure according to standard GB/T 1037 condition B, steam penetrating capacity is 6g/ ㎡ 24h, measures according to standard GB/T19789-2005 voltameter detection method, and the oxygen transit dose is 18g/ ㎡ 24h; Measure according to standard GB/T 5009.122-2003, do not detect residual vinylidene chloride monomer.
Embodiment 2
(1) mix monomer preparation: vinylidene chloride 91kg, ethyl acrylate 4.5kg, vinyl cyanide 0.5kg are mixed the rear 2h of stirring, for subsequent use;
(2) mixed polymerization emulsifying agent preparation: be after 1.2kg, 2A-1 emulsifying agent 1kg, methacrylic acid 4kg mix with COPS-1, thin up is to 20kg, and the high-speed stirring mixing is for subsequent use;
(3) initiator preparation: tertbutyl peroxide 80g, sodium formaldehyde sulphoxylate 80g are diluted to respectively mass percentage concentration are 2%, for subsequent use;
(4) Seeded polymerization: be that 280g adds in the 200L reactor with deionized water or soft water 64kg, auxiliary agent ammonium acetate 20g, iron protochloride 1g, seeding polymerization emulsifying agent Sodium dodecylbenzene sulfonate 120g, MA-80, the envelope still, with nitrogen replacement 3 times, vacuumize, suction 5%(weight) mix monomer that step 1 makes, cold dispersion 0.5h, be warming up to 47 ℃, speed with 8kg/48h is continuously pumped into the initiator for preparing, the control temperature of reaction is 55 ℃, when Pressure Drop during to 0.01-0.03MPa, seeding polymerization finishes, and obtains seed latex;
(5) letex polymerization: the speed that adds with 16h is continuously pumped into the remaining mix monomer that blending emulsifiers, step 1 that step 2 prepares make, when Pressure Drop to 0～-during 0.01MPa, reaction finishes, and adds microcrystalline wax 100g, vacuumize, bottom valve is not opened desorption 1h, and temperature rises to 70 ℃ and keeps 1h, and bottom valve is crack, desorption 2h, then the water vapor that adds 0.1MPa filters, and obtains copolymer emulsion.
Embodiment 3
(1) mix monomer preparation: vinylidene chloride 90kg, ethyl acrylate 5.7kg, vinyl cyanide 0.3kg are mixed the rear 2h of stirring, for subsequent use;
(2) mixed polymerization emulsifying agent preparation: be after 1.2kg, 2A-1 emulsifying agent 1kg, methacrylic acid 4kg mix with COPS-1, thin up is to 20kg, and the high-speed stirring mixing is for subsequent use;
(3) initiator preparation: tertbutyl peroxide 80g, sodium formaldehyde sulphoxylate 80g are diluted to respectively mass percentage concentration are 2%, for subsequent use;
(4) Seeded polymerization: be that 280g adds in the 200L reactor with deionized water or soft water 64kg, auxiliary agent ammonium acetate 20g, iron protochloride 1g, seeding polymerization emulsifying agent Sodium dodecylbenzene sulfonate 120g, MA-80, the envelope still, with nitrogen replacement 3 times, vacuumize, suction 5%(weight) mix monomer that step 1 makes, cold dispersion 0.5h, be warming up to 47 ℃, speed with 8kg/48h is continuously pumped into the initiator for preparing, the control temperature of reaction is 55 ℃, when Pressure Drop during to 0.01-0.03MPa, seeding polymerization finishes, and obtains seed latex;
(5) letex polymerization: the speed that adds with 16h is continuously pumped into the remaining mix monomer that blending emulsifiers, step 1 that step 2 prepares make, when Pressure Drop to 0～-during 0.01MPa, reaction finishes, and adds microcrystalline wax 100g, vacuumize, bottom valve is not opened desorption 1h, and temperature rises to 70 ℃ and keeps 1h, and bottom valve is crack, desorption 2h, then the water vapor that adds 0.1MPa filters, and obtains copolymer emulsion.
Claims (6)
1. a used for packing foods latex is characterized in that this latex is formed by the emulsion polymerization way copolymerization by following reaction raw materials, and reaction raw materials and weight part are:
(1) monomer mixture is 50 parts, and described monomer mixture comprises the vinylidene chloride, the ethyl acrylate that accounts for mix monomer gross weight 4-6% that account for mix monomer gross weight 89-91%, account for the vinyl cyanide of mix monomer gross weight 0.3-0.7% and account for the methacrylic acid of mix monomer gross weight 4-6%;
(2) initiator, described initiator comprises: organo-peroxide 0.04-0.12 part and sodium formaldehyde sulphoxylate 0.04-0.12 part;
(3) seeding polymerization emulsifying agent, described seeding polymerization emulsifying agent comprise that any one 0.06 part of being selected from the sodium sulfonate compounds and MA-80 are 0.14 part;
(4) blending emulsifiers, described blending emulsifiers comprise that it is 0.5 part with the 2A-1 emulsifying agent that COPS-1 is 0.6 part;
(5) auxiliary agent, described auxiliary agent comprise 0.0005 part of 0.012 part of ammonium acetate and iron protochloride.
2. used for packing foods latex according to claim 1 is characterized in that organo-peroxide is tertbutyl peroxide in the described initiator.
3. used for packing foods latex according to claim 1 is characterized in that the sodium sulfonate compounds is Sodium dodecylbenzene sulfonate in the described seeding polymerization emulsifying agent.
4. the preparation method of the described used for packing foods latex of arbitrary claim in 3 according to claim 1 is characterized in that adopting the preparation of seeding polymerization method, and concrete preparation process comprises:
(1) mix monomer preparation: described vinylidene chloride, ethyl acrylate, vinyl cyanide are mixed the rear 2h of stirring, for subsequent use;
(2) blending emulsifiers preparation: after described COPS-1,2A-1 emulsifying agent, methacrylic acid mixed, thin up to 10 part, the high-speed stirring mixing, for subsequent use;
(3) initiator preparation: described two kinds of initiators are diluted to respectively mass percentage concentration are 2%, for subsequent use;
(4) Seeded polymerization: deionized water or 32 parts of soft water, described auxiliary agent, described seeding polymerization emulsifying agent are added in the reactor, the envelope still is used nitrogen replacement 3 times, vacuumizes, suction accounts for the mix monomer of the mix monomer gross weight 5% that step 1 prepares, cold dispersion 0.5h is warming up to 47 ℃, is continuously pumped into the initiator for preparing with the speed of 8kg/48h, the control temperature of reaction is 55 ℃, when Pressure Drop during to 0.01-0.03MPa, seeding polymerization finishes, and obtains seed latex;
(5) letex polymerization: the speed that adds with 16h is continuously pumped into the remaining mix monomer that blending emulsifiers, step 1 that step 2 prepares make, when Pressure Drop to 0～-during 0.01MPa, reaction finishes, and adds microcrystalline wax, vacuumize, bottom valve is not opened desorption 1h, and temperature rises to 70 ℃ and keeps 1h, and bottom valve is crack, desorption 2h, then the water vapor that adds 0.1MPa filters, and obtains copolymer emulsion.
5. the according to claim 1 application of the described used for packing foods latex of arbitrary claim in the coating food packaging film in 3.
6. apply according to claim 1 the food product packing film of the described used for packing foods latex of arbitrary claim in 3.
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| CN1715559A (en) * | 2005-01-11 | 2006-01-04 | 东阳市野风塑胶有限公司 | Latex for coating drinking filter bag cotton paper and its preparing method |
| CN1986583A (en) * | 2006-12-07 | 2007-06-27 | 东阳市野风塑胶有限公司 | Water PVDC latex specially for painting special cloth and its preparing method |
| CN101186666A (en) * | 2007-11-19 | 2008-05-28 | 上海氯碱化工股份有限公司 | Method for preparing polyvinylidene chloride and acrylic ester copolymerization latex |
| CN101306743A (en) * | 2007-10-19 | 2008-11-19 | 河南双汇投资发展股份有限公司 | Packaging film for milk and method for manufacturing same |
| CN101613582A (en) * | 2009-07-23 | 2009-12-30 | 安徽大学 | The preparation method of aqueous vinylidene chloride base glue used in high-barrier plastic film |
| CN101649015A (en) * | 2009-08-27 | 2010-02-17 | 浙江野风塑胶有限公司 | Polyvinylidene chloride (PVDC) copolymer latex for medicine packaging as well as preparation method and application thereof |
| CN102650111A (en) * | 2012-05-10 | 2012-08-29 | 海南必凯水性涂料有限公司 | High-solid coating containing polyvinylidene chloride for paper coating and preparation method of coating |
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2012
- 2012-12-26 CN CN201210572303.1A patent/CN103044603B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1715559A (en) * | 2005-01-11 | 2006-01-04 | 东阳市野风塑胶有限公司 | Latex for coating drinking filter bag cotton paper and its preparing method |
| CN1986583A (en) * | 2006-12-07 | 2007-06-27 | 东阳市野风塑胶有限公司 | Water PVDC latex specially for painting special cloth and its preparing method |
| CN101306743A (en) * | 2007-10-19 | 2008-11-19 | 河南双汇投资发展股份有限公司 | Packaging film for milk and method for manufacturing same |
| CN101186666A (en) * | 2007-11-19 | 2008-05-28 | 上海氯碱化工股份有限公司 | Method for preparing polyvinylidene chloride and acrylic ester copolymerization latex |
| CN101613582A (en) * | 2009-07-23 | 2009-12-30 | 安徽大学 | The preparation method of aqueous vinylidene chloride base glue used in high-barrier plastic film |
| CN101649015A (en) * | 2009-08-27 | 2010-02-17 | 浙江野风塑胶有限公司 | Polyvinylidene chloride (PVDC) copolymer latex for medicine packaging as well as preparation method and application thereof |
| CN102650111A (en) * | 2012-05-10 | 2012-08-29 | 海南必凯水性涂料有限公司 | High-solid coating containing polyvinylidene chloride for paper coating and preparation method of coating |
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Application publication date: 20130417 Assignee: Hainan saigaoxin Material Co.,Ltd. Assignor: HAINAN BNK WATER-BASED NEW MATERIAL Co.,Ltd. Contract record no.: X2020980009604 Denomination of invention: Latex for food packaging and its preparation and Application Granted publication date: 20160316 License type: Common License Record date: 20201221 |