CN1102169C - Petroleum fermented nylon 1212 not-fusible colloid and its preparing process - Google Patents
Petroleum fermented nylon 1212 not-fusible colloid and its preparing process Download PDFInfo
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- CN1102169C CN1102169C CN99121120A CN99121120A CN1102169C CN 1102169 C CN1102169 C CN 1102169C CN 99121120 A CN99121120 A CN 99121120A CN 99121120 A CN99121120 A CN 99121120A CN 1102169 C CN1102169 C CN 1102169C
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Abstract
The present invention provides petroleum fermentation nylon 1212 hot melt adhesive. A petroleum fermentation nylon 1212 salt is used as a main component, and the components of a nylon 66 salt, an anti-aging agent, a molecular weight regulator, etc. are matched to synthesize the hot melt adhesive. The present invention simultaneously provides a preparation method for the hot melt adhesive. Compared with the prior art, the present invention has the advantages of low melting point and high bonding strength. The main component of the petroleum fermentation nylon 1212 salt of the present invention uses the light wax of a byproduct refined from petroleum as a raw material. Raw materials have abundant sources and low price. The hot melt adhesive has obvious superiority in the aspect of a raw material route, and has favorable market perspect.
Description
The present invention relates to the nylon hot-melt adhesive technical field.
Hot melt adhesive is to be the Hotmelt Adhesive of matrix component with the thermoplastic polymer, owing to be the fine powder that does not contain any solvent, just can be bonding rapidly firmly once hot pressing with adherend.It has safe, nuisanceless, accumulating convenient, can realize advantage such as mechanize high speed operation, thereby be a class tackiness agent with fastest developing speed over domestic and international 20 years.An important application of this hot melt adhesive is used for making the clothes adhesion lining cloth exactly.Use in the hot melt adhesive in whole Clothing industry, nylon (polymeric amide) is though the hot melt adhesive price is higher, but because of its cohesive force strong, snappiness is good, the wear resistance height, anti-dry-cleaning is outstanding, and fusing point lower (thereby the boiling hot temperature of required pressure is low), thereby development is very fast, becomes a current most important kind fabric hot melt adhesive both at home and abroad.In the nylon-type hot melt adhesive, the nylon hot-melt adhesive that contains long carbon chain nylon component (carbochain is 12), because its carbon chain length, so just increased carbochain length irregularity between component, also increased the gap of fusing point height between component, thereby reduced degree of crystallinity and fusing point effectively, again because the water-intake rate of long carbon chain nylon is low, help also that both anti-dry-cleaning is also water-fast washes, especially be suitable for the weather resistance lining cloth that high-grade clothing is used.Thereby the nylon hot-melt adhesive that contains the long carbon chain nylon component is the current domestic and international nylon hot-melt adhesive direction of development emphatically.
The present invention has carried out document Investigation with regard to relevant content, still find no the bibliographical information that closes petroleum fermented nylon 1212 not-fusible colloid, with the akin product of petroleum fermented nylon 1212 not-fusible colloid be nylon 12 hot melt adhesives, its preparation method following (reference: D.L.Bateman.HOT MELTADHESIVES.U.S.A.1978.):
Preparation nylon 12 hot melt adhesives used main raw material lauryl lactan, its synthesis step were at least for 6 steps, and step is longer, and because of the yield in each step all can not be very high, so its price is more expensive.Though its starting raw material divinyl through-stone oiling chemical product, but output is limited, and be used for the butylbenzene synthetic rubber of current maximum and output in a large number and occupy rubber such as deputy cis-1,4-polybutadiene rubber and neoprene, butyronitrile, only synthetic just supply falls short of demand for rubber, so the raw material supply anxiety.
It is abundant to the purpose of this invention is to provide a kind of raw material sources, and price is lower, and the long carbochain petroleum fermented nylon 1212 not-fusible colloid of superior performance and preparation method thereof.
To achieve these goals, the invention provides following technical scheme.
Petroleum fermented nylon 1212 not-fusible colloid is characterized in that each component concentration pass is: fermented petroleum nylon '1212 ' salt: nylon salt: hexanolactam; Anti-aging agent: molecular weight regulator: crystallization nucleating agent: white dyes=1: 0.3～1.8: 0.5～1.9: 0.05%～0.8%: 0.05%～5%: 0.03%～5%: 0.02%～3%.
The method for preparing petroleum fermented nylon 1212 not-fusible colloid is:
A, with fermented petroleum nylon '1212 ' salt, nylon salt, hexanolactam, anti-aging agent, molecular weight regulator, crystallization nucleating agent and white dyes by 1: 0.3～1.8: 0.5～1.9: 0.05%～0.8%: 0.05%～5%: 0.03%～5%: 0.02%～3% mixed, join in the polymeric kettle, vacuumized 5～20 minutes, make the interior vacuum tightness of still reach 0.01～0.002MPa, charge into CO again
2Gas to 0.05～0.1MPa, heat temperature raising then, when temperature rises to 200～250 ℃, the polymeric kettle internal pressure rises to 1.0～1.5MPa, and venting makes the still internal pressure begin to maintain 1.0～1.5MPa in 0.3～2.5 hour, after this accelerate venting speed, make the still internal pressure in 1.5～3.0 hours, reduce to normal pressure, under normal pressure, be incubated 0.5～3.0 hour, charge into CO
2Gas, pressure are 0.3～0.9MPa, open the discharging cock, and material flows out through the casting head, and cooling back pelletizing obtains the petroleum fermented nylon 1212 not-fusible colloid particle;
B, freezing crusher is dropped in petroleum fermented nylon 1212 not-fusible colloid particle oven dry back, in freezing crusher, inject liquid nitrogen, keep the interior hopper temperature of freezing crusher at-100 ℃～-190 ℃, opened refrigerator 0.5～5 hour, it is Powdered that the petroleum fermented nylon 1212 not-fusible colloid particle is ground into, and its particle size distribution is between 40 orders～400 orders;
C, the petroleum fermented nylon 1212 not-fusible colloid (Powdered) of above-mentioned size-grade distribution and lubricant are added in the trimmer in the evenly mixed back of 1: 0.01%～1.8% ratio, after the shaping 20～300 minutes, put into vacuum drying oven, drying is 0.5～10 hour in 60 ℃～120 ℃, promptly makes petroleum fermented nylon 1212 not-fusible colloid.
In above-mentioned hot melt adhesive, used anti-aging agent is a phosphorous acid; Molecular weight regulator is SL-AH or sebacic acid or hexanodioic acid or acetic acid; Crystallization nucleating agent is talcum powder or aluminum oxide or magnesium oxide or silicon-dioxide; White dyes is EBF or VBL.
In above-mentioned hot melt adhesive preparation method, lubricant is barium stearate or calcium stearate or aluminum stearate.
Compared with prior art, the present invention has the following advantages:
1, the present invention has superiority aspect raw material route
Main component lauryl lactan in domestic and international existing nylon 12 hot melt adhesives is to be starting raw material with the divinyl, though divinyl through-stone oiling chemical product, but output is limited, and be used for butylbenzene synthetic rubber and the deputy cis-1,4-polybutadiene rubber of output tool and the nitrile rubber of current output maximum in a large number, only rubber is synthetic is that supply falls short of demand, therefore must open up new raw material route.And the present invention is to be main component with nylon 1212 salt, cooperates other component synthetic, and fermented petroleum nylon '1212 ' salt is to pay the light wax (C of product with refining of petroleum
10～C
14Normal alkane) be raw material, because CNPC mostly is paraffinic base (alkyl) oil, contain a large amount of wax, and paraffin must be taken off again when refining oil product, so the source is very abundant, price is also cheap relatively.
2, the present invention has superiority aspect structure properties
Fabric requires snappiness good (good hand touch) with nylon hot-melt adhesive, and do not make the dress material damaged, thereby necessary degree of crystallinity is less, fusing point lower (so just not needing higher pressure to scald temperature), necessary in addition cohesive strength height, promptly anti-dry-cleaning is water-fast again washes, and the general requirement fusing point is better between 105～125 ℃, for fur then require 70～90 ℃ better, the method that reduces fusing point and degree of crystallinity generally is to adopt the copolymer nylon that contains long carbochain and short carbon chain nylon component.What adopt both at home and abroad is copolymer nylon 12/66/6, and the present invention's employing is copolymer nylon 1212/66/6.Owing to contain Ni Long11 11 salt and nylon 1313 salt about 1% in the main component fermented petroleum nylon '1212 ' salt in the petroleum fermented nylon 1212 not-fusible colloid, so just increased the irregularity of carbochain length between component, also increased the gap of fusing point height between component, thereby degree of crystallinity and fusing point have been reduced effectively, so the fusing point of petroleum fermented nylon 1212 not-fusible colloid lower (the boiling hot temperature of pressure is just low like this), and cohesive strength is higher.Thereby under the same conditions, petroleum fermented nylon 1212 not-fusible colloid is better than nylon 12 hot melt adhesives aspect structure properties.
Embodiment:
The first step, with 10kg fermented petroleum nylon '1212 ' salt, nylon salt, hexanolactam, anti-aging agent, molecular weight regulator, crystallization nucleating agent and white dyes by 1: 0.95: 1.1: 0.001: 0.005: 0.002: join in the polymeric kettle after 0.0004 the mixed, after vacuumizing, fill CO
2Gas begins heating, and when temperature rose to 220 ℃, system pressure reached 1.15MPa, begins venting, makes the still internal pressure maintain 1.0～1.1MPa in 1.5 hours in beginning, in 3 hours the still internal pressure is put to normal pressure then, and insulation charged into CO after 0.5 hour under normal pressure
2Gas, pressure are 0.6MPa, open the discharging cock, and material flows out through the casting head, and cooling back pelletizing promptly makes the petroleum fermented nylon 1212 not-fusible colloid particle.
Second step, the above-mentioned petroleum fermented nylon 1212 not-fusible colloid particle 40kg that in batches makes is put into freezing crusher, charge into liquid nitrogen, the temperature in the control refrigerator is about-120 ℃, under this temperature, pulverize, promptly make the petroleum fermented nylon 1212 not-fusible colloid powder.
The 3rd step, with above-mentioned every crowd of 30kg of petroleum fermented nylon 1212 not-fusible colloid powder that makes, add lubricant, make nylon hot-melt adhesive: lubricant is to put in trimmer at 1: 0.0008, shaping 20 minutes is put in the vacuum drier again and, handles after sieve after 4 hours in 70 ℃ of bakings, the particle size distribution that makes the hot melt adhesive powder promptly makes petroleum fermented nylon 1212 not-fusible colloid between 40 orders～200 orders.
Claims (4)
1, petroleum fermented nylon 1212 not-fusible colloid is characterized in that each component concentration pass is:
Fermented petroleum nylon '1212 ' salt: nylon salt: hexanolactam: anti-aging agent: molecular weight regulator: crystallization nucleating agent: white dyes=1: 0.3～1.8: 0.5～1.9: 0.05%～0.8%: 0.05%～5%: 0.03%～5%: 0.02%～3%.
2, the preparation method of petroleum fermented nylon 1212 not-fusible colloid is characterized in that:
A, with fermented petroleum nylon '1212 ' salt, nylon salt, hexanolactam, anti-aging agent, molecular weight regulator, crystallization nucleating agent and white dyes by 1: 0.3～1.8: 0.5～1.9: 0.05%～0.8%: 0.05%～5%: 0.03%～5%: 0.02%～3% mixed, join in the polymeric kettle, vacuumized 5～20 minutes, make the interior vacuum tightness of still reach 0.01～0.002MPa, charge into CO again
2Gas to 0.05～0.1MPa, heat temperature raising then, when temperature rises to 200～250 ℃, the polymeric kettle internal pressure rises to 1.0～1.5MPa, and venting makes the still internal pressure begin to maintain 1.0～1.5MPa in 0.3～2.5 hour, after this accelerate venting speed, make the still internal pressure in 1.5～3.0 hours, reduce to normal pressure, under normal pressure, be incubated 0.5～3.0 hour, charge into CO
2Gas, pressure are 0.3～0.9MPa, open the discharging cock, and material flows out through the casting head, and cooling back pelletizing obtains the petroleum fermented nylon 1212 not-fusible colloid particle;
B, freezing crusher is dropped in petroleum fermented nylon 1212 not-fusible colloid particle oven dry back, in freezing crusher, inject liquid nitrogen, keep the interior hopper temperature of freezing crusher at-100 ℃～-190 ℃, opened refrigerator 0.5～5 hour, it is Powdered that the petroleum fermented nylon 1212 not-fusible colloid particle is ground into, and its particle size distribution is between 40 orders～400 orders;
C, the Powdered hot melt adhesive of the fermented petroleum nylon '1212 ' of above-mentioned size-grade distribution and lubricant are added in the trimmer in the evenly mixed back of 1: 0.01%～1.8% ratio, after the shaping 20～300 minutes, put into vacuum drying oven, drying is 0.5～10 hour in 60 ℃～120 ℃, promptly makes petroleum fermented nylon 1212 not-fusible colloid.
3, according to the described petroleum fermented nylon 1212 not-fusible colloid of claim 1, it is characterized in that: anti-aging agent is a phosphorous acid, molecular weight regulator is SL-AH or sebacic acid or hexanodioic acid or acetic acid, crystallization nucleating agent is talcum powder or aluminum oxide or magnesium oxide or silicon-dioxide, and white dyes is EBF or VBL.
4, according to the preparation method of the described petroleum fermented nylon 1212 not-fusible colloid of claim 2, it is characterized in that: lubricant is barium stearate or calcium stearate or aluminum stearate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99121120A CN1102169C (en) | 1999-09-29 | 1999-09-29 | Petroleum fermented nylon 1212 not-fusible colloid and its preparing process |
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| Application Number | Priority Date | Filing Date | Title |
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| CN99121120A CN1102169C (en) | 1999-09-29 | 1999-09-29 | Petroleum fermented nylon 1212 not-fusible colloid and its preparing process |
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| Publication Number | Publication Date |
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| CN1283662A CN1283662A (en) | 2001-02-14 |
| CN1102169C true CN1102169C (en) | 2003-02-26 |
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| CN99121120A Expired - Fee Related CN1102169C (en) | 1999-09-29 | 1999-09-29 | Petroleum fermented nylon 1212 not-fusible colloid and its preparing process |
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| CN102925098A (en) * | 2012-11-29 | 2013-02-13 | 昆山天洋热熔胶有限公司 | Fast-melting polyamide powder hot melt adhesive and preparation method thereof |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS596220A (en) * | 1982-07-01 | 1984-01-13 | Daicel Chem Ind Ltd | New polyamide copolymer |
| CN1044664A (en) * | 1989-02-01 | 1990-08-15 | 河北工学院 | The manufacture method of polyesteramide thermosol for fabric |
| JPH06158018A (en) * | 1992-11-26 | 1994-06-07 | Nippon Synthetic Chem Ind Co Ltd:The | Hot-melt adhesive |
| JPH07157743A (en) * | 1993-12-06 | 1995-06-20 | Toray Ind Inc | Hot-melt type adhesive |
| CN1121101A (en) * | 1994-10-19 | 1996-04-24 | 中国石油化工总公司抚顺石油化工研究院 | Polyamide hot-melt adhesive and its prepn. method |
| CN1157643A (en) * | 1994-08-09 | 1997-08-20 | 旭化成工业株式会社 | Adhesive padding cloth, method of manufacturing same and bonding agent for adhesive cloths |
| EP0875534A1 (en) * | 1997-05-02 | 1998-11-04 | Dsm N.V. | Thermoplastic elastomer composition adhesion to polar materials |
| CN1215746A (en) * | 1997-10-28 | 1999-05-05 | 四川省大邑热缩制品厂 | Thermal state high strength hot melt adhesive with polyamide or polyester amide structure |
| JPH11124558A (en) * | 1997-10-23 | 1999-05-11 | Toagosei Co Ltd | Solution adhesive |
-
1999
- 1999-09-29 CN CN99121120A patent/CN1102169C/en not_active Expired - Fee Related
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS596220A (en) * | 1982-07-01 | 1984-01-13 | Daicel Chem Ind Ltd | New polyamide copolymer |
| CN1044664A (en) * | 1989-02-01 | 1990-08-15 | 河北工学院 | The manufacture method of polyesteramide thermosol for fabric |
| JPH06158018A (en) * | 1992-11-26 | 1994-06-07 | Nippon Synthetic Chem Ind Co Ltd:The | Hot-melt adhesive |
| JPH07157743A (en) * | 1993-12-06 | 1995-06-20 | Toray Ind Inc | Hot-melt type adhesive |
| CN1157643A (en) * | 1994-08-09 | 1997-08-20 | 旭化成工业株式会社 | Adhesive padding cloth, method of manufacturing same and bonding agent for adhesive cloths |
| CN1121101A (en) * | 1994-10-19 | 1996-04-24 | 中国石油化工总公司抚顺石油化工研究院 | Polyamide hot-melt adhesive and its prepn. method |
| EP0875534A1 (en) * | 1997-05-02 | 1998-11-04 | Dsm N.V. | Thermoplastic elastomer composition adhesion to polar materials |
| JPH11124558A (en) * | 1997-10-23 | 1999-05-11 | Toagosei Co Ltd | Solution adhesive |
| CN1215746A (en) * | 1997-10-28 | 1999-05-05 | 四川省大邑热缩制品厂 | Thermal state high strength hot melt adhesive with polyamide or polyester amide structure |
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| CN1283662A (en) | 2001-02-14 |
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