CN110317610A - A kind of preparation method and its manufacture system with low-volatile spheroidal antioxidant particle - Google Patents
A kind of preparation method and its manufacture system with low-volatile spheroidal antioxidant particle Download PDFInfo
- Publication number
- CN110317610A CN110317610A CN201910695539.6A CN201910695539A CN110317610A CN 110317610 A CN110317610 A CN 110317610A CN 201910695539 A CN201910695539 A CN 201910695539A CN 110317610 A CN110317610 A CN 110317610A
- Authority
- CN
- China
- Prior art keywords
- antioxidant
- butyl
- tert
- phenyl
- spheroidal
- Prior art date
- 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.)
- Pending
Links
- 239000003963 antioxidant agent Substances 0.000 title claims abstract description 122
- 230000003078 antioxidant effect Effects 0.000 title claims abstract description 122
- 239000002245 particle Substances 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 title abstract description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 188
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 94
- 239000002994 raw material Substances 0.000 claims abstract description 37
- 238000001816 cooling Methods 0.000 claims abstract description 29
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 7
- 239000007921 spray Substances 0.000 claims description 53
- 239000000470 constituent Substances 0.000 claims description 40
- -1 2,4- di-tert-butyl-phenyl Chemical group 0.000 claims description 36
- 238000009835 boiling Methods 0.000 claims description 28
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 21
- 230000008569 process Effects 0.000 claims description 21
- 238000005507 spraying Methods 0.000 claims description 21
- 238000011010 flushing procedure Methods 0.000 claims description 20
- 239000000155 melt Substances 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 18
- 239000012943 hotmelt Substances 0.000 claims description 17
- 235000019260 propionic acid Nutrition 0.000 claims description 13
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 11
- UAUDZVJPLUQNMU-KTKRTIGZSA-N erucamide Chemical compound CCCCCCCC\C=C/CCCCCCCCCCCC(N)=O UAUDZVJPLUQNMU-KTKRTIGZSA-N 0.000 claims description 11
- 239000002250 absorbent Substances 0.000 claims description 10
- 230000002745 absorbent Effects 0.000 claims description 10
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 claims description 10
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 claims description 10
- 229960001545 hydrotalcite Drugs 0.000 claims description 10
- 229910001701 hydrotalcite Inorganic materials 0.000 claims description 10
- 239000000314 lubricant Substances 0.000 claims description 10
- 239000002667 nucleating agent Substances 0.000 claims description 10
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical class OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 10
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 10
- 239000006096 absorbing agent Substances 0.000 claims description 9
- 239000004611 light stabiliser Substances 0.000 claims description 8
- RGASRBUYZODJTG-UHFFFAOYSA-N 1,1-bis(2,4-ditert-butylphenyl)-2,2-bis(hydroxymethyl)propane-1,3-diol dihydroxyphosphanyl dihydrogen phosphite Chemical class OP(O)OP(O)O.C(C)(C)(C)C1=C(C=CC(=C1)C(C)(C)C)C(O)(C(CO)(CO)CO)C1=C(C=C(C=C1)C(C)(C)C)C(C)(C)C RGASRBUYZODJTG-UHFFFAOYSA-N 0.000 claims description 7
- QUAMTGJKVDWJEQ-UHFFFAOYSA-N octabenzone Chemical compound OC1=CC(OCCCCCCCC)=CC=C1C(=O)C1=CC=CC=C1 QUAMTGJKVDWJEQ-UHFFFAOYSA-N 0.000 claims description 7
- XITRBUPOXXBIJN-UHFFFAOYSA-N bis(2,2,6,6-tetramethylpiperidin-4-yl) decanedioate Chemical compound C1C(C)(C)NC(C)(C)CC1OC(=O)CCCCCCCCC(=O)OC1CC(C)(C)NC(C)(C)C1 XITRBUPOXXBIJN-UHFFFAOYSA-N 0.000 claims description 6
- 150000002148 esters Chemical class 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- IKEHOXWJQXIQAG-UHFFFAOYSA-N 2-tert-butyl-4-methylphenol Chemical class CC1=CC=C(O)C(C(C)(C)C)=C1 IKEHOXWJQXIQAG-UHFFFAOYSA-N 0.000 claims description 5
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 5
- 239000012964 benzotriazole Substances 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000009472 formulation Methods 0.000 claims description 5
- 239000001384 succinic acid Substances 0.000 claims description 5
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 5
- NQRYJNQNLNOLGT-UHFFFAOYSA-N tetrahydropyridine hydrochloride Natural products C1CCNCC1 NQRYJNQNLNOLGT-UHFFFAOYSA-N 0.000 claims description 5
- 125000001841 imino group Chemical group [H]N=* 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- VNQNXQYZMPJLQX-UHFFFAOYSA-N 1,3,5-tris[(3,5-ditert-butyl-4-hydroxyphenyl)methyl]-1,3,5-triazinane-2,4,6-trione Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CN2C(N(CC=3C=C(C(O)=C(C=3)C(C)(C)C)C(C)(C)C)C(=O)N(CC=3C=C(C(O)=C(C=3)C(C)(C)C)C(C)(C)C)C2=O)=O)=C1 VNQNXQYZMPJLQX-UHFFFAOYSA-N 0.000 claims description 3
- VSAWBBYYMBQKIK-UHFFFAOYSA-N 4-[[3,5-bis[(3,5-ditert-butyl-4-hydroxyphenyl)methyl]-2,4,6-trimethylphenyl]methyl]-2,6-ditert-butylphenol Chemical compound CC1=C(CC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)C(C)=C(CC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)C(C)=C1CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 VSAWBBYYMBQKIK-UHFFFAOYSA-N 0.000 claims description 3
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims description 3
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 2
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims description 2
- 125000002777 acetyl group Chemical class [H]C([H])([H])C(*)=O 0.000 claims description 2
- FQUNFJULCYSSOP-UHFFFAOYSA-N bisoctrizole Chemical compound N1=C2C=CC=CC2=NN1C1=CC(C(C)(C)CC(C)(C)C)=CC(CC=2C(=C(C=C(C=2)C(C)(C)CC(C)(C)C)N2N=C3C=CC=CC3=N2)O)=C1O FQUNFJULCYSSOP-UHFFFAOYSA-N 0.000 claims description 2
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 2
- 239000008116 calcium stearate Substances 0.000 claims description 2
- 235000013539 calcium stearate Nutrition 0.000 claims description 2
- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 claims description 2
- FATBGEAMYMYZAF-UHFFFAOYSA-N oleicacidamide-heptaglycolether Natural products CCCCCCCCC=CCCCCCCCC(N)=O FATBGEAMYMYZAF-UHFFFAOYSA-N 0.000 claims description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 2
- 239000000600 sorbitol Substances 0.000 claims description 2
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 2
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 2
- UWSMKYBKUPAEJQ-UHFFFAOYSA-N 5-Chloro-2-(3,5-di-tert-butyl-2-hydroxyphenyl)-2H-benzotriazole Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC(N2N=C3C=C(Cl)C=CC3=N2)=C1O UWSMKYBKUPAEJQ-UHFFFAOYSA-N 0.000 claims 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- 159000000013 aluminium salts Chemical class 0.000 claims 1
- 229910000329 aluminium sulfate Inorganic materials 0.000 claims 1
- 238000009833 condensation Methods 0.000 claims 1
- 230000005494 condensation Effects 0.000 claims 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims 1
- ZPIRTVJRHUMMOI-UHFFFAOYSA-N octoxybenzene Chemical compound CCCCCCCCOC1=CC=CC=C1 ZPIRTVJRHUMMOI-UHFFFAOYSA-N 0.000 claims 1
- 229910052698 phosphorus Inorganic materials 0.000 claims 1
- 239000011574 phosphorus Substances 0.000 claims 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims 1
- 230000006641 stabilisation Effects 0.000 claims 1
- 238000011105 stabilization Methods 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 15
- 239000006185 dispersion Substances 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 238000006073 displacement reaction Methods 0.000 description 16
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 239000008187 granular material Substances 0.000 description 4
- KGRVJHAUYBGFFP-UHFFFAOYSA-N 2,2'-Methylenebis(4-methyl-6-tert-butylphenol) Chemical compound CC(C)(C)C1=CC(C)=CC(CC=2C(=C(C=C(C)C=2)C(C)(C)C)O)=C1O KGRVJHAUYBGFFP-UHFFFAOYSA-N 0.000 description 3
- 239000003595 mist Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000000889 atomisation Methods 0.000 description 2
- 150000003851 azoles Chemical class 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 125000005605 benzo group Chemical group 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- HEJCZAMFVMNFLC-UHFFFAOYSA-N 10-oxo-10-(2,2,6,6-tetramethylpiperidin-4-yl)oxydecanoic acid Chemical compound CC1(C)CC(OC(=O)CCCCCCCCC(O)=O)CC(C)(C)N1 HEJCZAMFVMNFLC-UHFFFAOYSA-N 0.000 description 1
- AGGKHDYTKZAPRA-UHFFFAOYSA-N 2,4-ditert-butyl-6-(4-chlorophenyl)phenol Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC(C=2C=CC(Cl)=CC=2)=C1O AGGKHDYTKZAPRA-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 239000000110 cooling liquid Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- YFSFQQIYYPVYPL-UHFFFAOYSA-N n-(2,4,4-trimethylpentan-2-yl)-1,3,5-triazin-2-amine Chemical compound CC(C)(C)CC(C)(C)N=C1N=CN=CN1 YFSFQQIYYPVYPL-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 150000008301 phosphite esters Chemical class 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K15/00—Anti-oxidant compositions; Compositions inhibiting chemical change
- C09K15/04—Anti-oxidant compositions; Compositions inhibiting chemical change containing organic compounds
- C09K15/06—Anti-oxidant compositions; Compositions inhibiting chemical change containing organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K15/00—Anti-oxidant compositions; Compositions inhibiting chemical change
- C09K15/04—Anti-oxidant compositions; Compositions inhibiting chemical change containing organic compounds
- C09K15/06—Anti-oxidant compositions; Compositions inhibiting chemical change containing organic compounds containing oxygen
- C09K15/08—Anti-oxidant compositions; Compositions inhibiting chemical change containing organic compounds containing oxygen containing a phenol or quinone moiety
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K15/00—Anti-oxidant compositions; Compositions inhibiting chemical change
- C09K15/04—Anti-oxidant compositions; Compositions inhibiting chemical change containing organic compounds
- C09K15/30—Anti-oxidant compositions; Compositions inhibiting chemical change containing organic compounds containing heterocyclic ring with at least one nitrogen atom as ring member
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K15/00—Anti-oxidant compositions; Compositions inhibiting chemical change
- C09K15/04—Anti-oxidant compositions; Compositions inhibiting chemical change containing organic compounds
- C09K15/32—Anti-oxidant compositions; Compositions inhibiting chemical change containing organic compounds containing two or more of boron, silicon, phosphorus, selenium, tellurium or a metal
- C09K15/322—Anti-oxidant compositions; Compositions inhibiting chemical change containing organic compounds containing two or more of boron, silicon, phosphorus, selenium, tellurium or a metal containing only phosphorus
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention belongs to antioxidant and its composite forming technology fields, use fusing point for 30-300 DEG C of antioxidant more particularly to a kind of, or the ball-shaped antioxidant particle that the functional aid for using fusing point to be 10~300 DEG C for 30~300 DEG C of antioxidant and fusing point is prepared as a raw material, cooling by nitrogen reduces product temperature, the volatile matter of abjection is set to liquefy to reduce the volatile matter and its manufacture system of product to the cold.The present invention has the preparation method and its manufacture system of low-volatile spheroidal antioxidant particle, and product particle dispersion, epigranular and volatile matter are low, and several functions auxiliary agent is mixed together with antioxidant, volatile matter can be reduced simultaneously, save human and material resources.
Description
Technical field
The invention belongs to the technologies of preparing of antioxidant and its complexing agent particle, and in particular to one kind has low-volatile circle
The preparation method and its manufacture system of spherical antioxidant particle.
Background technique
Antioxidant particle has many advantages, such as do not have convenient for storage, convenient transportation, and in use relative to powder
Powder formulation is also easy to produce the puzzlements such as dust pollution, the agglomerating and wall built-up of coalescence, and particle has more relative to powder in actual use
High dispersibility；While particle especially spherical granules have more relative to sheet or the band-like equal biggish antioxidant of particles
Good dispersibility can greatly reduce the uneven situation of mixing subsequent in use, be conducive to preferably control dosage and proportion.
Since the preparation process of itself can introduce volatile component, the antioxidant raw material containing high volatile is added antioxidant raw material
In the plate used at one's side to people, use feeling will affect, or even have some impact on to the health of people.
Summary of the invention
Invention broadly provides a kind of preparation methods and its manufacture with low-volatile spheroidal antioxidant particle
System, cooling by nitrogen reduce product temperature, and the volatile matter of abjection is made to liquefy to reduce the volatile matter of product to the cold.Its
Technical solution is as follows:
A kind of preparation method with low-volatile spheroidal antioxidant particle, which is characterized in that the antioxidant
Use fusing point for 30-300 DEG C of antioxidant, or using fusing point for 30~300 DEG C of antioxidant and fusing point is 10~300 DEG C
Functional aid be prepared as a raw material；It is characterized in that, the granularity of the antioxidant particle is 0.2~2.5mm；It is made
Preparation Method includes the following steps,
(1) raw material is placed in heating fusing in the hot melt kettle after nitrogen is replaced and stirred；
(2) it when the melt dynamic viscosity of step (1) is in 1~20mPa.s, is pumped in the spray distributor of spray tower and sprays
Mist, under 5~50KPa pressure, droplet passes through the upper nitrogen flushing air cooling of 5~20 DEG C of 0.1~1m/s in high tower drip process
It is dry, obtain spheroidal antioxidant particle；
(3) spheroidal antioxidant is placed in boiling machine and further removes fugitive constituent with 0~10 DEG C of nitrogen, obtain low wave
Send out part spheroidal antioxidant；
(4) by the fugitive constituent removed in step (3) as nitrogen carries out -20 DEG C of cryogenic liquefying.
Further, antioxidant described in step (1) was four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] seasons
Doutrate, phosphorous acid three (2,4- di-tert-butyl-phenyl) ester, 3- (3,5- di-tert-butyl-hydroxy phenyl) propionic acid n-octadecane
Alcohol ester, 1,3,5- tri- (3,5- di-tert-butyl-4-hydroxyl benzyl) isocyanuric acid, bis- (2,4- di-tert-butyl-phenyl) pentaerythrites two
Phosphite ester, 2,2' methylene bis (4- methyl-6-tert-butylphenol) and (the tertiary fourth of 3,5- bis- of 1,3,5- trimethyl 2,4,6- tri-
Base -4- hydroxybenzyl) one of benzene or a variety of.
Specifically, when the raw material used in step (1) is four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] season penta
When four alcohol esters, the heating temperature is 160~210 DEG C and speed of agitator is 80~90rpm；
When the raw material used in step (1) is phosphorous acid three (2,4- di-tert-butyl-phenyl) ester, the heating temperature is
200~235 DEG C and speed of agitator are 90~100rpm；
When the raw material used in step (1) is 3- (3,5- di-tert-butyl-hydroxy phenyl) propionic acid n-octadecane alcohol ester,
The heating temperature is 85~120 DEG C and speed of agitator is 60~70rpm；
The raw material used in the step (1) is 1, when 3,5- tri- (3,5- di-tert-butyl-4-hydroxyl benzyl) isocyanuric acid, institute
State that heating temperature is 250~270 DEG C and speed of agitator is 100~110rpm；
It is described when the raw material used in step (1) is bis- (2,4- di-tert-butyl-phenyl) pentaerythritol diphosphites
Heating temperature is 100~125 DEG C and speed of agitator is 60~70rpm；
When the raw material used in step (1) is 2,2'- di-2-ethylhexylphosphine oxide (4- methyl-6-tert-butylphenol), the heating
Temperature is 160~185 DEG C and speed of agitator is 70~80rpm；
The antioxidant described in step (1) is (3,5- di-t-butyl -4- hydroxyl benzyl of 1,3,5- trimethyl 2,4,6- tri-
Base) benzene when, the heating temperature is 265~275 DEG C and speed of agitator is 110~120rpm.
Further, in the step (1) raw material by 45~85% fusing points be 30~300 DEG C antioxidant and 15~
The functional aid that 55% fusing point is 10~300 DEG C forms.
Further, the functional aid includes the ultraviolet radiation absorption for accounting for functional aid total weight 0~6% respectively
Agent, 0~9% light stabilizer, 10~15% lubricant, 50~75% acid absorbent and 15~30% nucleating agent.
Further, the ultraviolet absorbing agent selects [2- hydroxyl -4- (octyloxy) phenyl] phenyl ketone, 2- (2'- hydroxyl
Base -3'- tert-butyl -5'- aminomethyl phenyl) -5- chlorobenzotriazole, 2- (2'- hydroxyl -3', 5'- di-tert-butyl phenyl) -5- chlorobenzene
And triazole, 2- (bis- tertiary amyl phenyl of 2'- hydroxyl -3', 5'-) benzotriazole, 2- (2'- hydroxyl -5'- spy octyl phenyl) benzo three
Azoles, 2,2' methylene bis (4- t-octyl -6- benzotriazole phenol), 2- [bis- (the 2,4- xylyl) -2- (1,3,5- tri- of 2,4-
Piperazine base) any one in 5- phenol octyloxy；The light stabilizer selects bis- (2,2,6,6- tetramethyl -4- piperidyl) last of the ten Heavenly stems two
Acid esters, the condensate of succinic acid and 4- hydroxyl -2,2,6,6- tetramethyl -1- piperidine alcohols, poly- { [6- [(1,1,3,3- tetramethyl butyl)
Amino]] -1,3,5- triazine -2,4- [(2,2,6,6,-tetramethyl-4-piperidyl) imino group] -1,6- oneself two support [(2,2,6,6- tetra-
Methyl -4- piperidyl) imino group] in any one；The lubricant is using any in erucyl amide, oleamide
It is a kind of；The acid absorbent is room temperature solid formulation, using any one in calcium stearate, zinc stearate, hydrotalcite；The nucleation
Agent is room temperature solid formulation, using 1,3:2,4- bis- (3,4- dimethyl) benzylidene sorbitol acetal, 2,2 '-di-2-ethylhexylphosphine oxides (4,6- bis-
Tert-butyl benzene oxygroup) any one in phosphalugel.
Specifically, working as antioxidant in raw material is 3- (3,5- di-tert-butyl-hydroxy phenyl) propionic acid n-octadecane alcohol ester
When, ultraviolet absorbing agent described in the functional aid of raw material uses 2- (bis- tertiary amyl phenyl of 2'- hydroxyl -3', 5'-) benzo three
Azoles；The light stabilizer uses the condensate of succinic acid and 4- hydroxyl -2,2,6,6- tetramethyl -1- piperidine alcohols；The lubricant is adopted
Use erucyl amide；The acid absorbent uses hydrotalcite；The nucleating agent uses 2,2 '-di-2-ethylhexylphosphine oxides (4,6- di-tert-butyl oxygen
Base) phosphalugel；The heating temperature is 105~120 DEG C and speed of agitator is 60~70rpm；
When antioxidant is bis- (2,4- di-tert-butyl-phenyl) pentaerythritol diphosphites in raw material, the function of raw material
Property auxiliary agent described in ultraviolet absorbing agent use [2- hydroxyl -4- (octyloxy) phenyl] phenyl ketone；The light stabilizer is using double
(2,2,6,6- tetramethyl -4- piperidyl) sebacate；The lubricant uses erucyl amide；The acid absorbent uses neatly
Stone；The nucleating agent uses 2,2 '-di-2-ethylhexylphosphine oxides (4,6- di-t-butyl phenoxy group) phosphalugel；The heating temperature is 100
~125 DEG C and speed of agitator are 60~70rpm；
When antioxidant is 2,2'- di-2-ethylhexylphosphine oxide (4- methyl-6-tert-butylphenol) in raw material, the functionality of raw material is helped
Ultraviolet absorbing agent described in agent uses [2- hydroxyl -4- (octyloxy) phenyl] phenyl ketone；The light stabilizer using it is bis- (2,2,
6,6- tetramethyl -4- piperidyl) sebacate；The lubricant uses erucyl amide；The acid absorbent uses hydrotalcite；It is described
Nucleating agent uses 2,2 '-di-2-ethylhexylphosphine oxides (4,6- di-t-butyl phenoxy group) phosphalugel；The heating temperature is 160~185 DEG C
And speed of agitator is 70~80rpm.
A kind of manufacture system of the particle of ball-shaped antioxidant and the compound other function auxiliary agent of antioxidant, feature
It is, including heat exchanger, condenser, hot melt kettle, spray tower and boiling machine；Vacuum pump and nitrogen are connected at the top of the hot melt kettle
Motor-driven valve；The discharge port of the hot melt kettle bottom side is connect with the spray tower top side by pipeline；The spray tower
The top other side is equipped with air outlet, and bottom is equipped with air inlet fan and discharge port；The air outlet and discharge port of the spray tower pass through pipe
Road is successively connect with the first circulation blower and the boiling machine；The air outlet of the boiling machine is connected in turn by pipeline
Cyclone separator, demister, the first condenser and second circulation blower；The outlet of the condenser passes through pipeline and the nitrogen
Motor-driven valve connection；The nitrogen motor-driven valve is connect by pipeline with the heat exchanger；The air outlet of the heat exchanger simultaneously with institute
State air inlet and the connection of the second condenser of spray tower；The air inlet of the air outlet of second condenser and the boiling machine and
The connection of third condenser；The air outlet of the third condenser is connected with cooling tower.
Using the above scheme, the method for the present invention has the advantage that
The present invention is blow molded by low temperature nitrogen, and antioxidant is made into spherical granules shape, particle dispersion and epigranular,
In the subsequent use process, it is more advantageous to and is uniformly mixed and dosage control；Raw material is subjected to melting mixing in hot melt kettle, it is former
The volatile matter contained in material largely volatilizees at high temperature, and carries out cooling liquid with the circulation temperature lowering of nitrogen and collect, and can save
About cost while, greatly reduce the volatile matter in product, improve the safety of product, use is more healthy；By multiple functions
Property auxiliary agent mixes together with antioxidant, can directly be counted according to raw material proportioning when can reduce volatile matter and later period use simultaneously
The content for calculating each auxiliary agent does not need to carry out independent measurement and addition to each auxiliary agent, saves manpower, and can reduce repeatedly addition and make
At the uneven problem of dosage inaccuracy and mixing.
Detailed description of the invention
Fig. 1 is the flow chart of the manufacture system of ball-shaped antioxidant particle of the present invention
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1
(1) four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters are placed in the heat after nitrogen displacement
200 DEG C are heated in molten kettle and with the stirring of 80~90rpm speed；
(2) when the melt dynamic viscosity of step (1) is in 8mPa.s, be pumped in the spray distributor of spray tower it is spraying,
Under 30KPa pressure, the upper nitrogen flushing air cooling of 0.1~1m/s of the droplet in high tower drip process by 10 DEG C is dry, obtains circle
Spherical antioxidant particle；
(3) spheroidal antioxidant is placed in boiling machine, further removes fugitive constituent in 5 DEG C of nitrogen streams, obtains low wave
Send out part spheroidal antioxidant particle；
(4) by the fugitive constituent removed in step (3) as nitrogen carries out -20 DEG C of cryogenic liquefying.
Embodiment 2
(1) phosphorous acid three (2,4- di-tert-butyl-phenyl) ester is placed in the hot melt kettle after nitrogen is replaced and is heated to 220 DEG C
And with the stirring of 90~100rpm speed；
(2) when the melt dynamic viscosity of step (1) is in 8mPa.s, be pumped in the spray distributor of spray tower it is spraying,
Under 30KPa pressure, the upper nitrogen flushing air cooling of 0.1~1m/s of the droplet in high tower drip process by 10 DEG C is dry, obtains circle
Spherical composite antioxidant particle；
(3) spheroidal antioxidant is placed in boiling machine, further removes fugitive constituent in 5 DEG C of nitrogen streams, obtains low wave
Send out part spheroidal composite antioxidant particle；
(4) by the fugitive constituent removed in step (3) as nitrogen carries out -20 DEG C of cryogenic liquefying.
Embodiment 3
(1) 3- (3,5- di-tert-butyl-hydroxy phenyl) propionic acid n-octadecane alcohol ester is placed in the hot melt after nitrogen displacement
110 DEG C are heated in kettle and with the stirring of 60~70rpm speed；
(2) when the melt dynamic viscosity of step (1) is in 8mPa.s, be pumped in the spray distributor of spray tower it is spraying,
Under 30KPa pressure, the upper nitrogen flushing air cooling of 0.1~1m/s of the droplet in high tower drip process by 10 DEG C is dry, obtains circle
Spherical composite antioxidant particle；
(3) spheroidal antioxidant is placed in boiling machine, further removes fugitive constituent in 5 DEG C of nitrogen streams, obtains low wave
Send out part spheroidal composite antioxidant particle；
(4) by the fugitive constituent removed in step (3) as nitrogen carries out -20 DEG C of cryogenic liquefying.
Embodiment 4
(1) 1,3,5- tri- (3,5- di-tert-butyl-4-hydroxyl benzyl) isocyanuric acid is placed in the hot melt kettle after nitrogen displacement
In be heated to 250 DEG C and with 100~110rpm speed stirring；
(2) when the melt dynamic viscosity of step (1) is in 8mPa.s, be pumped in the spray distributor of spray tower it is spraying,
Under 30KPa pressure, the upper nitrogen flushing air cooling of 0.1~1m/s of the droplet in high tower drip process by 10 DEG C is dry, obtains circle
Spherical composite antioxidant particle；
(3) spheroidal antioxidant is placed in boiling machine, further removes fugitive constituent in 5 DEG C of nitrogen streams, obtains low wave
Send out part spheroidal composite antioxidant particle；
(4) by the fugitive constituent removed in step (3) as nitrogen carries out -20 DEG C of cryogenic liquefying.
Embodiment 5
(1) will be bis- (2,4- di-tert-butyl-phenyl) pentaerythritol diphosphites be placed in nitrogen displacement after hot melt kettle in plus
Heat is to 110 DEG C and with the stirring of 60~70rpm speed；
(2) when the melt dynamic viscosity of step (1) is in 1mPa.s, be pumped in the spray distributor of spray tower it is spraying,
Under 30KPa pressure, the upper nitrogen flushing air cooling of 0.1~1m/s of the droplet in high tower drip process by 10 DEG C is dry, obtains circle
Spherical composite antioxidant particle；
(3) spheroidal antioxidant is placed in boiling machine, further removes fugitive constituent in 5 DEG C of nitrogen streams, obtains low wave
Send out part spheroidal composite antioxidant particle；
(4) by the fugitive constituent removed in step (3) as nitrogen carries out -20 DEG C of cryogenic liquefying.
Embodiment 6
(1) 2,2' methylene bis (4- methyl-6-tert-butylphenol) is placed in the hot melt kettle after nitrogen is replaced and is heated to
170 DEG C and with 70~80rpm speed stirring；
(2) it when the melt dynamic viscosity of step (1) is in 100mPa.s, is pumped in the spray distributor of spray tower and sprays
Mist, under 30KPa pressure, the upper nitrogen flushing air cooling of 0.1~1m/s of the droplet in high tower drip process by 10 DEG C is dry, obtains
Spheroidal composite antioxidant particle；
(3) spheroidal antioxidant is placed in boiling machine, further removes fugitive constituent in 5 DEG C of nitrogen streams, obtains low wave
Send out part spheroidal composite antioxidant particle；
(4) by the fugitive constituent removed in step (3) as nitrogen carries out -20 DEG C of cryogenic liquefying.
Embodiment 7
(1) after 1,3,5- trimethyl 2,4,6- tri- (3,5- di-tert-butyl-4-hydroxyl benzyl) benzene being placed in nitrogen displacement
265 DEG C are heated in hot melt kettle and with the stirring of 110~120rpm speed；
(2) when the melt dynamic viscosity of step (1) is in 8mPa.s, be pumped in the spray distributor of spray tower it is spraying,
Under 5KPa pressure, the upper nitrogen flushing air cooling of 0.1~1m/s of the droplet in high tower drip process by 10 DEG C is dry, obtains ball
Shape composite antioxidant particle；
(3) spheroidal antioxidant is placed in boiling machine, further removes fugitive constituent in 5 DEG C of nitrogen streams, obtains low wave
Send out part spheroidal composite antioxidant particle；
(4) by the fugitive constituent removed in step (3) as nitrogen carries out -20 DEG C of cryogenic liquefying.
Embodiment 8
(1) four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters are placed in the heat after nitrogen displacement
200 DEG C are heated in molten kettle and with the stirring of 80~90rpm speed；
(2) when the melt dynamic viscosity of step (1) is in 1mPa.s, be pumped in the spray distributor of spray tower it is spraying,
Under 30KPa pressure, the upper nitrogen flushing air cooling of 0.1~1m/s of the droplet in high tower drip process by 10 DEG C is dry, obtains circle
Spherical antioxidant particle；
(3) spheroidal antioxidant is placed in boiling machine, further removes fugitive constituent in 5 DEG C of nitrogen streams, obtains low wave
Send out part spheroidal antioxidant particle；
(4) by the fugitive constituent removed in step (3) as nitrogen carries out -20 DEG C of cryogenic liquefying.
Embodiment 9
(1) four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters are placed in the heat after nitrogen displacement
200 DEG C are heated in molten kettle and with the stirring of 80~90rpm speed；
(2) when the melt dynamic viscosity of step (1) is in 20mPa.s, be pumped in the spray distributor of spray tower it is spraying,
Under 30KPa pressure, the upper nitrogen flushing air cooling of 0.1~1m/s of the droplet in high tower drip process by 10 DEG C is dry, obtains circle
Spherical antioxidant particle；
(3) spheroidal antioxidant is placed in boiling machine, further removes fugitive constituent in 5 DEG C of nitrogen streams, obtains low wave
Send out part spheroidal antioxidant particle；
(4) by the fugitive constituent removed in step (3) as nitrogen carries out -20 DEG C of cryogenic liquefying.
Embodiment 10
(1) four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters are placed in the heat after nitrogen displacement
200 DEG C are heated in molten kettle and with the stirring of 80~90rpm speed；
(2) when the melt dynamic viscosity of step (1) is in 20mPa.s, be pumped in the spray distributor of spray tower it is spraying,
Under 5KPa pressure, the upper nitrogen flushing air cooling of 0.1~1m/s of the droplet in high tower drip process by 10 DEG C is dry, obtains ball
Shape antioxidant particle；
(3) spheroidal antioxidant is placed in boiling machine, further removes fugitive constituent in 5 DEG C of nitrogen streams, obtains low wave
Send out part spheroidal antioxidant particle；
(4) by the fugitive constituent removed in step (3) as nitrogen carries out -20 DEG C of cryogenic liquefying.
Embodiment 11
(1) four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters are placed in the heat after nitrogen displacement
200 DEG C are heated in molten kettle and with the stirring of 80~90rpm speed；
(2) when the melt dynamic viscosity of step (1) is in 20mPa.s, be pumped in the spray distributor of spray tower it is spraying,
Under 50KPa pressure, the upper nitrogen flushing air cooling of 0.1~1m/s of the droplet in high tower drip process by 10 DEG C is dry, obtains circle
Spherical antioxidant particle；
(3) spheroidal antioxidant is placed in boiling machine, further removes fugitive constituent in 5 DEG C of nitrogen streams, obtains low wave
Send out part spheroidal antioxidant particle；
(4) by the fugitive constituent removed in step (3) as nitrogen carries out -20 DEG C of cryogenic liquefying.
Embodiment 12
(1) four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters are placed in the heat after nitrogen displacement
200 DEG C are heated in molten kettle and with the stirring of 80~90rpm speed；
(2) when the melt dynamic viscosity of step (1) is in 20mPa.s, be pumped in the spray distributor of spray tower it is spraying,
Under 30KPa pressure, the upper nitrogen flushing air cooling of 0.1~1m/s of the droplet in high tower drip process by 5 DEG C is dry, obtains ball
Shape antioxidant particle；
(3) spheroidal antioxidant is placed in boiling machine, further removes fugitive constituent in 5 DEG C of nitrogen streams, obtains low wave
Send out part spheroidal antioxidant particle；
(4) by the fugitive constituent removed in step (3) as nitrogen carries out -20 DEG C of cryogenic liquefying.
Embodiment 13
(1) four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters are placed in the heat after nitrogen displacement
200 DEG C are heated in molten kettle and with the stirring of 80~90rpm speed；
(2) when the melt dynamic viscosity of step (1) is in 20mPa.s, be pumped in the spray distributor of spray tower it is spraying,
Under 30KPa pressure, the upper nitrogen flushing air cooling of 0.1~1m/s of the droplet in high tower drip process by 20 DEG C is dry, obtains circle
Spherical antioxidant particle；
(3) spheroidal antioxidant is placed in boiling machine, further removes fugitive constituent in 5 DEG C of nitrogen streams, obtains low wave
Send out part spheroidal antioxidant particle；
(4) by the fugitive constituent removed in step (3) as nitrogen carries out -20 DEG C of cryogenic liquefying.
Embodiment 14
(1) four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters are placed in the heat after nitrogen displacement
200 DEG C are heated in molten kettle and with the stirring of 80~90rpm speed；
(2) when the melt dynamic viscosity of step (1) is in 20mPa.s, be pumped in the spray distributor of spray tower it is spraying,
Under 30KPa pressure, the upper nitrogen flushing air cooling of 0.1~1m/s of the droplet in high tower drip process by 10 DEG C is dry, obtains circle
Spherical antioxidant particle；
(3) spheroidal antioxidant is placed in boiling machine, further removes fugitive constituent in 0 DEG C of nitrogen stream, obtains low wave
Send out part spheroidal antioxidant particle；
(4) by the fugitive constituent removed in step (3) as nitrogen carries out -20 DEG C of cryogenic liquefying.
Embodiment 15
(1) four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters are placed in the heat after nitrogen displacement
200 DEG C are heated in molten kettle and with the stirring of 80~90rpm speed；
(2) when the melt dynamic viscosity of step (1) is in 20mPa.s, be pumped in the spray distributor of spray tower it is spraying,
Under 30KPa pressure, the upper nitrogen flushing air cooling of 0.1~1m/s of the droplet in high tower drip process by 10 DEG C is dry, obtains circle
Spherical antioxidant particle；
(3) spheroidal antioxidant is placed in boiling machine, further removes fugitive constituent in 10 DEG C of nitrogen streams, obtains low wave
Send out part spheroidal antioxidant particle；
(4) by the fugitive constituent removed in step (3) as nitrogen carries out -20 DEG C of cryogenic liquefying.
Embodiment 16
(1) by account for total mass of raw material 75% 3- (3,5- di-tert-butyl-hydroxy phenyl) propionic acid n-octadecane alcohol ester,
0.5% 2- (bis- tertiary amyl phenyl of 2'- hydroxyl -3', 5'-) benzotriazole, 0.5% succinic acid and 4- hydroxyl -2,2,6,6-
The condensate of tetramethyl -1- piperidine alcohols, 3% erucyl amide, 16.5% hydrotalcite and the 2,2 ' of 4.5%-di-2-ethylhexylphosphine oxide (4,6-
Di-t-butyl phenoxy group) it is heated to 110 DEG C and is stirred with 60~70rpm speed in the hot melt kettle that is placed in after nitrogen displacement of phosphalugel
It mixes；
(2) when the melt dynamic viscosity of step (1) is in 8mPa.s, be pumped in the spray distributor of spray tower it is spraying,
Under 30KPa pressure, the upper nitrogen flushing air cooling of 0.1~1m/s of the droplet in high tower drip process by 10 DEG C is dry, obtains circle
Spherical antioxidant particle；
(3) spheroidal antioxidant is placed in boiling machine, further removes fugitive constituent in 5 DEG C of nitrogen streams, obtains low wave
Send out part spheroidal antioxidant particle；
(4) by the fugitive constituent removed in step (3) as nitrogen carries out -20 DEG C of cryogenic liquefying.
Embodiment 17
(1) by account for total mass of raw material 45% bis- (2,4- di-tert-butyl-phenyl) pentaerythritol diphosphites, 2%
[2- hydroxyl -4- (octyloxy) phenyl] phenyl ketone, 3% bis(2,2,6,6-tetramethyl-4-piperidyl)sebacate, 7%
Erucyl amide, 32% hydrotalcite and the 2,2 ' of 11%-di-2-ethylhexylphosphine oxides (4,6- di-t-butyl phenoxy group) phosphalugel are placed in nitrogen
110 DEG C are heated in hot melt kettle after gas displacement and with the stirring of 60~70rpm speed；
(2) when the melt dynamic viscosity of step (1) is in 8mPa.s, be pumped in the spray distributor of spray tower it is spraying,
Under 30KPa pressure, the upper nitrogen flushing air cooling of 0.1~1m/s of the droplet in high tower drip process by 10 DEG C is dry, obtains circle
Spherical antioxidant particle；
(3) spheroidal antioxidant is placed in boiling machine, further removes fugitive constituent in 5 DEG C of nitrogen streams, obtains low wave
Send out part spheroidal antioxidant particle；
(4) by the fugitive constituent removed in step (3) as nitrogen carries out -20 DEG C of cryogenic liquefying.
Embodiment 18
(1) by 85% 2,2' methylene bis (4- methyl-6-tert-butylphenol), 0.2% [2- hydroxyl -4- (pungent oxygen
Base) phenyl] phenyl ketone, 0.3% bis(2,2,6,6-tetramethyl-4-piperidyl)sebacate, 1% erucyl amide, 9.5%
Hydrotalcite and 4% 2,2 '-di-2-ethylhexylphosphine oxides (4,6- di-t-butyl phenoxy group) phosphalugel be placed in nitrogen displacement after hot melt kettle
In be heated to 170 DEG C and with 70~80rpm speed stirring；
(2) when the melt dynamic viscosity of step (1) is in 8mPa.s, be pumped in the spray distributor of spray tower it is spraying,
Under 30KPa pressure, the upper nitrogen flushing air cooling of 0.1~1m/s of the droplet in high tower drip process by 10 DEG C is dry, obtains circle
Spherical antioxidant particle；
(3) spheroidal antioxidant is placed in boiling machine, further removes fugitive constituent in 5 DEG C of nitrogen streams, obtains low wave
Send out part spheroidal antioxidant particle；
(4) by the fugitive constituent removed in step (3) as nitrogen carries out -20 DEG C of cryogenic liquefying.
Embodiment product form and volatile matter content compare:
Various embodiments of the present invention measure volatile matter according to the regulation of GB/T 11409.4, are analyzed by above-described embodiment 1~18
As can be seen that the volatile matter content of measurement is significantly lower than the volatile matter content of each antioxidant product national Specification, and all
For evengranular spherical granules.
Examples 1 to 7 is the Granulation Example of different antioxidant particles, can be analyzed by upper table, different antioxidant particles
Granularity is both less than 1.0mm, and particle is uniform, and volatile matter content is 0.2% hereinafter, the higher antioxidant of partial melting temperature is waved
Hair point content is slightly below the low antioxidant of melting temperature；Embodiment 8~15 is antioxidant of the same race making under the conditions of differential responses
Grain embodiment, as can be seen from the above table, within the scope of granulating system and method for the invention, the volatile matter content of antioxidant particle
Between 0.1~0.15%, content is lower and stablizes, and in the range of preparation method of the invention, dynamic viscosity increases, sprays
The temperature of the reduction of mist pressure and cooling nitrogen, which is got higher, can make antioxidant grain diameter of the invention slightly become larger；Dynamic viscosity subtracts
The temperature of small, atomisation pressure increase and cooling nitrogen is lower and grain diameter can be made to become smaller.It is real in the actual production of the present inventor
It in testing, is reduced to when dynamic viscosity and by spraying more than limitation range of the invention, then particle can be excessive, or even makes to spraying ejection
At influence, make particle adhesion, volatile matter cannot be cooled down well to which content increases；Dynamic viscosity reduces, the drop of atomisation pressure
As low as being more than that limitation range of the invention can make spraying ejection excessively violent, drop not yet comes into full contact with cooling nitrogen and just drops down onto
Bottom can be such that particle not yet cooling and shaping change completely falls if the temperature of cooling nitrogen is increased to more than limitation range of the invention
Under, the adhesion of particle is caused, product effect is influenced.
Embodiment 16~18 is the Granulation Example of the antioxidant and composite functional builder granule of different ratio and content,
As can be seen from the above table, the antioxidant particle volatile matter content for being compounded with functional aid is still lower than 0.2%, and melting temperature is high
Antioxidant particle volatile matter content be slightly below the low antioxidant of melting temperature；Composite antioxidant particle overall shape is regular, all
For spheroidal, and it is of moderate size；The high antioxidant grain diameter of compound functional aid content slightly becomes larger, poor partial size
Slightly become smaller.
It will be apparent to those skilled in the art that can make various other according to the above description of the technical scheme and ideas
Corresponding change and deformation, and all these changes and deformation all should belong to the protection scope of the claims in the present invention
Within.
Claims (8)
1. a kind of preparation method with low-volatile spheroidal antioxidant particle, the antioxidant use fusing point for 30-
300 DEG C of antioxidant, or use the functional aid that fusing point is 10~300 DEG C for 30~300 DEG C of antioxidant and fusing point
It is prepared as a raw material；It is characterized in that, the granularity of the antioxidant particle is 0.2~2.5mm；Preparation method include with
Lower step,
(1) raw material is placed in heating fusing in the hot melt kettle after nitrogen is replaced and stirred；
(2) when the melt dynamic viscosity of step (1) is in 1~20mPa.s, be pumped in the spray distributor of spray tower it is spraying,
Under 5~50KPa pressure, the upper nitrogen flushing air cooling of 0.1~1m/s of the droplet in high tower drip process by 5~20 DEG C is dry
It is dry, obtain spheroidal antioxidant particle；
(3) spheroidal antioxidant is placed in boiling machine and further removes fugitive constituent with 0~10 DEG C of nitrogen, obtain low-volatile
Spheroidal antioxidant；
(4) by the fugitive constituent removed in step (3) as nitrogen carries out -20 DEG C of cryogenic liquefying.
2. the preparation method according to claim 1 with low-volatile spheroidal antioxidant particle, which is characterized in that
Antioxidant described in step (1) is four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters, phosphorous acid three
(2,4- di-tert-butyl-phenyl) ester, 3- (3,5- di-tert-butyl-hydroxy phenyl) propionic acid n-octadecane alcohol ester, 1,3,5- tri- (3,
5- di-tert-butyl-4-hydroxyl benzyl) isocyanuric acid, bis- (2,4- di-tert-butyl-phenyl) pentaerythritol diphosphites, the Asia 2,2'-
Methyl bis- (4- methyl-6-tert-butylphenols) and 1,3,5- trimethyl 2,4,6- tri- (3,5- di-tert-butyl-4-hydroxyl benzyl) benzene
One of or it is a variety of.
3. the preparation method according to claim 1 or 2 with low-volatile spheroidal antioxidant particle, feature exist
In,
When the raw material used in step (1) is four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, institute
State that heating temperature is 160~210 DEG C and speed of agitator is 80~90rpm；
When the raw material used in the step (1) is phosphorous acid three (2,4- di-tert-butyl-phenyl) ester, the heating temperature for 200~
235 DEG C and speed of agitator are 90~100rpm；
It is described when the raw material used in step (1) is 3- (3,5- di-tert-butyl-hydroxy phenyl) propionic acid n-octadecane alcohol ester
Heating temperature is 85~120 DEG C and speed of agitator is 60~70rpm；
The raw material used in the step (1) is 1, described to add when 3,5- tri- (3,5- di-tert-butyl-4-hydroxyl benzyl) isocyanuric acid
Hot temperature is 250~270 DEG C and speed of agitator is 100~110rpm；
When the raw material used in step (1) is bis- (2,4- di-tert-butyl-phenyl) pentaerythritol diphosphites, the heating
Temperature is 170~195 DEG C and speed of agitator is 60~70rpm；
When the raw material used in step (1) is 2,2'- di-2-ethylhexylphosphine oxide (4- methyl-6-tert-butylphenol), the heating temperature
For 160~185 DEG C and speed of agitator is 70~80rpm；
The antioxidant described in step (1) is 1,3,5- trimethyl 2,4,6- tri- (3,5- di-tert-butyl-4-hydroxyl benzyl) benzene
When, the heating temperature is 265~275 DEG C and speed of agitator is 110~120rpm.
4. the preparation method according to claim 1 or 2 with low-volatile spheroidal antioxidant particle, feature exist
In, the antioxidant and 15~55% fusing points that raw material is 30~300 DEG C by 45~85% fusing points in the step (1) be 10~
300 DEG C of functional aid composition.
5. the preparation method according to claim 4 with low-volatile spheroidal antioxidant particle, which is characterized in that
The functional aid includes the light stabilization of the ultraviolet absorbing agent for accounting for functional aid total weight 0~6% respectively, 0~9%
Agent, 10~15% lubricant, 50~75% acid absorbent and 15~30% nucleating agent.
6. the preparation method according to claim 5 with low-volatile spheroidal antioxidant particle, which is characterized in that
The ultraviolet absorbing agent selects [2- hydroxyl -4- (octyloxy) phenyl] phenyl ketone, 2- (2'- hydroxyl -3'- tert-butyl -5'- first
Base phenyl) -5- chlorobenzotriazole, 2- (2'- hydroxyl -3', 5'- di-tert-butyl phenyl) -5- chlorobenzotriazole, 2- (2'- hydroxyl -
Bis- tertiary amyl phenyl of 3', 5'-) benzotriazole, 2- (2'- hydroxyl -5'- spy octyl phenyl) benzotriazole, 2,2' methylene bis
(4- t-octyl -6- benzotriazole phenol), 2- [2,4- bis- (2,4- xylyls) -2- (cyanuro 1,3,5) 5- octyloxy benzene
Any one in phenol；The light stabilizer selects bis(2,2,6,6-tetramethyl-4-piperidyl)sebacate, succinic acid and 4-
The condensate of hydroxyl -2,2,6,6- tetramethyl -1- piperidine alcohols, poly- { [6- [(1,1,3,3- tetramethyl butyl) amino]] -1,3,5- three
Piperazine -2,4- [(2,2,6,6,-tetramethyl-4-piperidyl) imino group] -1,6- oneself two support [(2,2,6,6- tetramethyl -4- piperidyl)
Imino group] } in any one；The lubricant is using any one in erucyl amide, oleamide；The acid absorbent
For room temperature solid formulation, using any one in calcium stearate, zinc stearate, hydrotalcite；The nucleating agent is room temperature solid formulation,
Using 1,3:2,4- bis- (3,4- dimethyl) benzylidene sorbitol acetal, 2,2 '-di-2-ethylhexylphosphine oxides (4,6- di-t-butyl phenoxy group) phosphorus
Any one in sour aluminium salt.
7. according to claim 1, with the preparation method of low-volatile spheroidal antioxidant particle, feature described in 2 or 6
It is,
When antioxidant is 3- (3,5- di-tert-butyl-hydroxy phenyl) propionic acid n-octadecane alcohol ester in raw material, the function of raw material
Ultraviolet absorbing agent described in energy property auxiliary agent uses 2- (bis- tertiary amyl phenyl of 2'- hydroxyl -3', 5'-) benzotriazole；The light is steady
Determine the condensate that agent uses succinic acid and 4- hydroxyl -2,2,6,6- tetramethyl -1- piperidine alcohols；The lubricant uses erucyl amide；
The acid absorbent uses hydrotalcite；The nucleating agent uses 2,2 '-di-2-ethylhexylphosphine oxides (4,6- di-t-butyl phenoxy group) phosphalugel；
The heating temperature is 105~120 DEG C and speed of agitator is 60~70rpm；
When antioxidant is bis- (2,4- di-tert-butyl-phenyl) pentaerythritol diphosphites in raw material, the functionality of raw material is helped
Ultraviolet absorbing agent described in agent uses [2- hydroxyl -4- (octyloxy) phenyl] phenyl ketone；The light stabilizer using it is bis- (2,2,
6,6- tetramethyl -4- piperidyl) sebacate；The lubricant uses erucyl amide；The acid absorbent uses hydrotalcite；It is described
Nucleating agent uses 2,2 '-di-2-ethylhexylphosphine oxides (4,6- di-t-butyl phenoxy group) phosphalugel；The heating temperature is 100~125 DEG C
And speed of agitator is 60~70rpm；
When antioxidant is 2,2'- di-2-ethylhexylphosphine oxide (4- methyl-6-tert-butylphenol) in raw material, in the functional aid of raw material
The ultraviolet absorbing agent uses [2- hydroxyl -4- (octyloxy) phenyl] phenyl ketone；The light stabilizer uses bis- (2,2,6,6-
Tetramethyl -4- piperidyl) sebacate；The lubricant uses erucyl amide；The acid absorbent uses hydrotalcite；The nucleation
Agent uses 2,2 '-di-2-ethylhexylphosphine oxides (4,6- di-t-butyl phenoxy group) phosphalugel；The heating temperature is 160~185 DEG C and stirs
Mixing revolving speed is 70~80rpm.
8. a kind of preparation system for preparation method described in claim 1, which is characterized in that including heat exchanger, condenser, heat
Molten kettle, spray tower and boiling machine；Vacuum pump and nitrogen motor-driven valve are connected at the top of the hot melt kettle；The hot melt kettle bottom side
Discharge port connect with the spray tower top side by pipeline；The other side is equipped with air outlet, bottom at the top of the spray tower
Equipped with air inlet fan and discharge port；The air outlet of the spray tower and discharge port by pipeline successively with the first circulation blower and
The boiling machine connection；The air outlet of the boiling machine is connected with cyclone separator, demister, the first condensation in turn by pipeline
Device and second circulation blower；The outlet of the condenser is connect by pipeline with the nitrogen motor-driven valve；The nitrogen motor-driven valve
It is connect by pipeline with the heat exchanger；The air outlet of the heat exchanger is condensed with the air inlet of the spray tower and second simultaneously
Device connection；The air outlet of second condenser is connected to the air inlet of the boiling machine and third condenser；The third is cold
The air outlet of condenser is connected with cooling tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910695539.6A CN110317610A (en) | 2019-07-30 | 2019-07-30 | A kind of preparation method and its manufacture system with low-volatile spheroidal antioxidant particle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910695539.6A CN110317610A (en) | 2019-07-30 | 2019-07-30 | A kind of preparation method and its manufacture system with low-volatile spheroidal antioxidant particle |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110317610A true CN110317610A (en) | 2019-10-11 |
Family
ID=68124936
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910695539.6A Pending CN110317610A (en) | 2019-07-30 | 2019-07-30 | A kind of preparation method and its manufacture system with low-volatile spheroidal antioxidant particle |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110317610A (en) |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1280591A (en) * | 1997-11-12 | 2001-01-17 | 纳幕尔杜邦公司 | Method for producing reactive coating powder compositions |
| CN1283222A (en) * | 1997-12-26 | 2001-02-07 | 日本钢管株式会社 | Refining method of molten iron and reduction smelting method for producing molten iron |
| CN1944511A (en) * | 2006-10-26 | 2007-04-11 | 上海金海雅宝精细化工有限公司 | Premixed composite granular antioxidant for polyolifen and its preparing method |
| CN101506329A (en) * | 2006-08-15 | 2009-08-12 | 科聚亚公司 | Antioxidants and methods of making antioxidants |
| CN105601998A (en) * | 2016-01-18 | 2016-05-25 | 佟立新 | Antioxidant in shape of bead-shaped particles and preparation method and application thereof |
| CN105968339A (en) * | 2015-03-10 | 2016-09-28 | 赢创德固赛有限公司 | Antioxidants for producing low-emission PUR systems |
| CN208166099U (en) * | 2018-04-11 | 2018-11-30 | 郑伟 | A kind of device adding antioxidant |
| CN109744455A (en) * | 2017-11-08 | 2019-05-14 | 丹阳市博元安全生产服务有限公司 | A kind of antioxidant |
| CN109825025A (en) * | 2019-01-22 | 2019-05-31 | 重庆鑫翎创福光电科技股份有限公司 | Outdoor furniture made from a kind of ABS composition, preparation method and combinations thereof |
| CN209076623U (en) * | 2018-11-15 | 2019-07-09 | 淄博万科化工有限公司 | Antioxidant prilling granulator |
-
2019
- 2019-07-30 CN CN201910695539.6A patent/CN110317610A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1280591A (en) * | 1997-11-12 | 2001-01-17 | 纳幕尔杜邦公司 | Method for producing reactive coating powder compositions |
| CN1283222A (en) * | 1997-12-26 | 2001-02-07 | 日本钢管株式会社 | Refining method of molten iron and reduction smelting method for producing molten iron |
| CN101506329A (en) * | 2006-08-15 | 2009-08-12 | 科聚亚公司 | Antioxidants and methods of making antioxidants |
| CN1944511A (en) * | 2006-10-26 | 2007-04-11 | 上海金海雅宝精细化工有限公司 | Premixed composite granular antioxidant for polyolifen and its preparing method |
| CN105968339A (en) * | 2015-03-10 | 2016-09-28 | 赢创德固赛有限公司 | Antioxidants for producing low-emission PUR systems |
| CN105601998A (en) * | 2016-01-18 | 2016-05-25 | 佟立新 | Antioxidant in shape of bead-shaped particles and preparation method and application thereof |
| CN109744455A (en) * | 2017-11-08 | 2019-05-14 | 丹阳市博元安全生产服务有限公司 | A kind of antioxidant |
| CN208166099U (en) * | 2018-04-11 | 2018-11-30 | 郑伟 | A kind of device adding antioxidant |
| CN209076623U (en) * | 2018-11-15 | 2019-07-09 | 淄博万科化工有限公司 | Antioxidant prilling granulator |
| CN109825025A (en) * | 2019-01-22 | 2019-05-31 | 重庆鑫翎创福光电科技股份有限公司 | Outdoor furniture made from a kind of ABS composition, preparation method and combinations thereof |
Non-Patent Citations (1)
| Title |
|---|
| 于树炎: "闭路循环在抗氧剂D L T P 喷雾冷却造粒中的应用", 《南京林业大学学报》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101423581B (en) | Soap-free core-shell emulsion type amphiphilic polymer resin and preparation and application thereof in preparation of function humidity controlling coating | |
| CN101701738B (en) | Fresh air handling unit for regulating humidity and controlling temperature by adopting solution and control method thereof | |
| CN206064437U (en) | A kind of humidity control device in climate compartment | |
| CN104226103B (en) | A kind of Indoor Air Formaldehyde scavenger based on air cooler application and purification method thereof | |
| CN102607108A (en) | Air purification device mainly relying on water spray dedusting and supplemented by water-cooling refrigeration dehumidification | |
| CN211800650U (en) | Pressure spray granulator | |
| CN110317610A (en) | A kind of preparation method and its manufacture system with low-volatile spheroidal antioxidant particle | |
| CN108654124A (en) | The device and method of volatile organic compounds in a kind of removing lotion | |
| CN106196990A (en) | Degree of depth dehumidifying unit in conjunction with cooling tower and heat pump | |
| CN201652662U (en) | A Direct Evaporative Cooling Air Conditioning Unit Combining High-Pressure Micro Mist and Packing | |
| CN107975898A (en) | One kind evaporates cold evaporated water control device and its control method | |
| CN206950706U (en) | Ventilating and cooling crystallizing tower | |
| CN104315624A (en) | Air-assisted atomization solution dehumidification air-conditioning system | |
| CN203190541U (en) | Air humidity adjusting system utilizing liquid moisture absorber | |
| CN201652658U (en) | Packing—high-pressure micro-mist composite direct evaporative cooling air conditioning unit | |
| WO2019068315A1 (en) | Gas humidity regulating method and regulator | |
| CN107062442A (en) | A kind of energy-saving air processing system | |
| CN207610306U (en) | A kind of cold evaporated water control device of evaporation | |
| CN117443139A (en) | Recycling method and recycling system for circulating return air type condensed NMP | |
| CN207317107U (en) | A kind of safety check instrument package AC plant | |
| CN103245015A (en) | Method for purifying air based on water spraying and supplemented by water-cooled refrigerating system | |
| CN206609076U (en) | A kind of energy-saving air processing system | |
| CN108224606B (en) | A kind of heat pump humidifier and working method | |
| CN206572702U (en) | A kind of energy-saving air processing system with secondary return air | |
| CN202216351U (en) | Atomizing cooling device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20191011 |