CN107722282A - A kind of elastomer silicone based on Vinyl MQ silicon resin and preparation method thereof - Google Patents
A kind of elastomer silicone based on Vinyl MQ silicon resin and preparation method thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/44—Block-or graft-polymers containing polysiloxane sequences containing only polysiloxane sequences
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/70—Siloxanes defined by use of the MDTQ nomenclature
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Abstract
The invention belongs to organosilicon material field, discloses a kind of elastomer silicone based on Vinyl MQ silicon resin and preparation method thereof.The preparation method is：50~100 DEG C are warming up to after hydrogen containing siloxane, Vinyl MQ silicon resin and carrier fluid are uniformly mixed, then add platinum catalyst, 0.5~10.0h of insulation reaction, products therefrom obtain the elastomer silicone based on Vinyl MQ silicon resin after high speed shear acts on.The present invention passes through hydrosilylation addition reaction with hydrogen containing siloxane and Vinyl MQ silicon resin, elastomer silicone is obtained in the direct cross-linking reaction of carrier fluid, the elastomer phase of products therefrom and traditional structure ratio, conventional elastomer gel, which can be significantly improved, has the shortcomings that greasy feeling, strengthen the silty sense of product, formula compatibility performance is lifted, skin is produced smooth but non-greasy sensation.
Description
Technical field
The invention belongs to organosilicon material field, and in particular to a kind of organosilicone elastic based on Vinyl MQ silicon resin
Body and preparation method thereof.
Background technology
Elastomer silicone material has the advantages that high-low temperature resistant, weather-proof, resistance to ozone, highly-breathable and physiological inertia,
In daily use chemicals industry, elastomer silicone typically presents and is clear to translucent gel, therefore also known as elastomer silicone coagulates
Glue.Have benefited from its unique cross-linked structure, elastomer silicone has certain resilience, work as painting when applying external force
Smear on skin, the change of its microstructure makes people's soft feel comfortable, there is velvet-like silk smooth felling.Therefore, organosilicon
Elastomer gel obtains the favor of cosmetics engineer, and often addition is in the cosmetics of super quality.
Silicone elastomer gels are usually to be dispersed to small molecule carrier by the macromolecule organic silica gel powder of cross-linking type
It is made in fluid, conventional preparation method is to block poly- silica using organic hydrogen polysiloxanes and straight chain type α, ω-bi-vinyl
Alkane or α, ω diene hydrocarbon reaction are made, such as：Patent of invention CN 106633076A report the Silicon Containing Hydrogen containing phenyl on main chain
Oil and the silicon gel that phenyl is carried in bi-vinyl silicone oil preparation structure；Patent of invention CN 102512339B have been reported
Machine hydrogen siloxane and unsaturated compound, silicon gel is prepared under platinum catalyst.Conventional small molecule carrier fluid has ten
Methyl D5 (D5), low viscosity methyl-silicone oil, isomery dodecane, hexamethylene etc..
MQ silicones is stereochemical structure organosilicon material of the molecule using Si-O keys as skeleton, has benefited from its long hammer
Shape molecular structure, there is good mechanical performance, film forming and heat-resisting quantity, be applied to liquid silicon rubber frequently as supporting material
Glue or packaging plastic material, Vinyl MQ silicon resin are then that the silicones of C=C double bonds is carried in structure.But rarely have MQ silicon at present
Resin is used for the report for preparing daily use chemicals silicone elastomer gels.
The content of the invention
In place of shortcoming and defect existing for above prior art, primary and foremost purpose of the invention is to provide a kind of base
In the elastomer silicone of Vinyl MQ silicon resin.
Another object of the present invention is to provide the preparation side of the above-mentioned elastomer silicone based on Vinyl MQ silicon resin
Method.
The object of the invention is achieved through the following technical solutions：
A kind of elastomer silicone based on Vinyl MQ silicon resin, is polymerize to obtain by following component cross-link：
A) hydrogen containing siloxane；
B) Vinyl MQ silicon resin；
C) platinum catalyst；
D) carrier fluid.
Preferably, the hydrogen containing siloxane is the dimethyl silicone polymer that side chain or end group contain Si -- H bond, and its H contains
Measure as 0.05~0.5wt.%, viscosity is 5.0~300.0cSt at its 25 DEG C.
Preferably, the Vinyl MQ silicon resin, its vinyl (CH2=CH-) content is 0.5~3.0wt.%, number is equal
Molecular weight is that 2000~10000, M/Q is 0.5~1.5.
Preferably, the platinum catalyst is the aqueous isopropanol or vinyl platinum complex of chloroplatinic acid.
Preferably, the carrier fluid refers to the ring-type or linear polydimethyl that viscosity is 1.0~50.0cSt at 25 DEG C
Siloxanes, the content of carrier fluid is 70~95wt.%.
The preparation method of the above-mentioned elastomer silicone based on Vinyl MQ silicon resin, including following preparation process：
50~100 are warming up to after hydrogen containing siloxane, Vinyl MQ silicon resin and carrier fluid are uniformly mixed
DEG C, platinum catalyst, 0.5~10.0h of insulation reaction are then added, products therefrom obtains being based on second after high speed shear acts on
The elastomer silicone of alkenyl MQ silicones.
Preferably, the molar ratio of C=C keys and Si -- H bond in hydrogen containing siloxane is C in the Vinyl MQ silicon resin
=C/Si-H=(1~2)/1.
Preferably, the addition of the platinum catalyst is calculated with concentration of the metal platinum in system, and metal platinum is in system
In concentration be 2~20ppm.
Preferably, the high speed shear effect refers to be handled using three-roller type grinder or colloid mill.
The present invention principle be：Contain M links, Q links and vinyl groups in the structure of Vinyl MQ silicon resin.This
Invention utilizes the C=C double bonds and Si-H in vinyl MQ silicones using MQ resins oil absorption is good, has the characteristics of silty sense
The addition reaction of key, prepare a kind of elastomer silicone cross-linked polymer of new structure, the elastomer phase with traditional structure
Than the polymer in the present invention can significantly improve the shortcomings that conventional elastomer gel greasy feeling is strong, strengthen the smooth feeling of product
And silty sense, formula compatibility performance is lifted, skin is produced smooth but non-greasy sensation.
The present invention preparation method and resulting product has the following advantages that and beneficial effect：
The present invention with hydrogen containing siloxane and Vinyl MQ silicon resin by hydrosilylation addition reaction, it is straight in carrier fluid
Connect cross-linking reaction and obtain the elastomer phase ratio of elastomer silicone, products therefrom and traditional structure, conventional elastomer can be improved
The shortcomings that gel greasy feeling is strong, strengthens the silty sense of product, lifts formula compatibility performance, produces skin soft smooth but not
Greasy sensation.
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Embodiment 1
It is that 0.05%, 25 DEG C of viscosity is 50.0cSt that 100.0g hydrogen contents are sequentially added in 1000mL four round flask
Hydrogen containing siloxane, 60.0g contents of ethylene is 0.5%, number-average molecular weight 3000, M/Q be 1.2 vinyl MQ silicon
Resin, both C=C/Si-H=1.2/1, then add 373.3g decamethylcyclopentaandoxanes (D5, 25 DEG C of viscosity are about
2.8cSt), carrier fluid content is 70%, opens mechanical agitation, is warming up to 80 DEG C, adds the chloroplatinic acid isopropanol of amount of calculation
Solution, the content for making metal platinum in system are 3ppm, and successive reaction 8.0h at such a temperature, then will react obtain it is solidifying
Glue passes through the effect of three-roller type grinder, obtains a kind of translucent gel-thickened compound, is elastomer silicone polymer 1.
Embodiment 2
It is that 0.1%, 25 DEG C of viscosity is 50.0 cSt that 100.0g hydrogen contents are sequentially added in 1000mL four round flask
Hydrogen containing siloxane, 33.3g contents of ethylene is 0.3%, number-average molecular weight 3000, M/Q be 1.2 vinyl MQ silicon
Resin, both C=C/Si-H=1/1, then add 533.2g decamethylcyclopentaandoxanes (D5, 25 DEG C of viscosity are about
2.8cSt), carrier fluid content is 80%, opens mechanical agitation, is warming up to 80 DEG C, adds the chloroplatinic acid isopropanol of amount of calculation
Solution, the content for making metal platinum in system are 3.0ppm, and successive reaction 8.0h at such a temperature, then will react what is obtained
Gel passes through the effect of three-roller type grinder, obtains a kind of translucent gel-thickened compound, is elastomer silicone polymer
2。
Embodiment 3
It is that 0.1%, 25 DEG C of viscosity is 300.0cSt that 100.0g hydrogen contents are sequentially added in 1000mL four round flask
Hydrogen containing siloxane, 36.6g contents of ethylene is 0.3%, number-average molecular weight 3000, M/Q be 1.2 vinyl MQ silicon
Resin, both C=C/Si-H=1.1/1, then add 533.2g decamethylcyclopentaandoxanes (D5, 25 DEG C of viscosity are about
2.8cSt), carrier fluid content is 80%, opens mechanical agitation, is warming up to 50 DEG C, adds the vinyl complexing platinum of amount of calculation
Catalyst, the content for making metal platinum in system are 20.0 ppm, and successive reaction 8.0h at such a temperature, then obtain reaction
Gel pass through three-roller type grinder effect, obtain a kind of translucent gel-thickened compound, for elastomer silicone polymerize
Thing 3.
Embodiment 4
It is that 0.3%, 25 DEG C of viscosity is 300.0cSt that 100.0g hydrogen contents are sequentially added in 1000mL four round flask
Hydrogen containing siloxane, 27.5g contents of ethylene is 1.2%, number-average molecular weight 2000, M/Q be 1.4 vinyl MQ silicon
Resin, both C=C/Si-H=1.1/1, it is about the poly- silica of 6.0cSt linear dimethyls then to add 25 DEG C of viscosity of 510.0g
Alkane, carrier fluid content are 80%, open mechanical agitation, are warming up to 70 DEG C, add the vinyl complexing platinum catalysis of amount of calculation
Agent, the content for making metal platinum in system are 4.0ppm, and successive reaction 8.0h at such a temperature, then will react obtain it is solidifying
Glue passes through the effect of three-roller type grinder, obtains a kind of translucent gel-thickened compound, is elastomer silicone polymer 4.
Embodiment 5
It is that 0.2%, 25 DEG C of viscosity is 150.0cSt that 100.0g hydrogen contents are sequentially added in 1000mL four round flask
Hydrogen containing siloxane, 7.3g contents of ethylene is 3.0%, number-average molecular weight 2000, M/Q be 1.5 vinyl MQ silicon tree
Fat, both C=C/Si-H=1.1/1, it is 50.0cSt linear dimethyl polysiloxanes then to add 25 DEG C of viscosity of 429.2g,
Carrier fluid content is 80%, opens mechanical agitation, is warming up to 70 DEG C, adds the vinyl complexing platinum catalyst of amount of calculation, makes
The content of metal platinum is 4.0ppm in system, and successive reaction 6.0h at such a temperature, the gel for then obtaining reaction pass through
The effect of three-roller type grinder, a kind of translucent gel-thickened compound is obtained, be elastomer silicone polymer 5.
Embodiment 6
It is that 0.5%, 25 DEG C of viscosity is 150 cSt that 40.0g hydrogen contents are sequentially added in 1000mL four round flask
Hydrogen containing siloxane, 4.8g contents of ethylene is 3.0%, number-average molecular weight 3000, and M/Q is 1.5 vinyl MQ silicon tree
Fat, both C=C/Si-H=2.0/1, it is 5.0cSt linear dimethyl polysiloxanes then to add 25 DEG C of viscosity of 179.2g, is carried
Body fluid content is 80%, opens mechanical agitation, is warming up to 70 DEG C, adds the vinyl complexing platinum catalyst of amount of calculation, makes body
The content of metal platinum is 4.0ppm in system, and successive reaction 10.0h at such a temperature, the gel for then obtaining reaction pass through
The effect of colloid mill, a kind of translucent gel-thickened compound is obtained, be elastomer silicone polymer 6.
Embodiment 7
It is that 0.2%, 25 DEG C of viscosity is 5.0 cSt that 25.0g hydrogen contents are sequentially added in 1000mL four round flask
Hydrogen containing siloxane, 5.0g contents of ethylene is 1.2%, number-average molecular weight 3000, and M/Q is 1.4 vinyl MQ silicon tree
Fat, both C=C/Si-H=1.2:1, it is 5.0cSt linear dimethyl polysiloxanes then to add 25 DEG C of viscosity of 570.0g, is carried
Body fluid content is 95%, opens mechanical agitation, is warming up to 80 DEG C, adds the vinyl complexing platinum catalyst of amount of calculation, makes body
The content of metal platinum is 4.0ppm in system, and successive reaction 8.0h at such a temperature, then will react obtained gel and passes through glue
The effect of body mill, obtains a kind of translucent gel-thickened compound, is named as elastomer silicone polymer 7.
Embodiment 8
It is that 0.1%, 25 DEG C of viscosity is 50.0 cSt that 100.0g hydrogen contents are sequentially added in 1000mL four round flask
Hydrogen containing siloxane, 24.0g contents of ethylene is 0.5%, number-average molecular weight 10000, M/Q be 0.7 vinyl MQ silicon
Resin, both C=C/Si-H=1.2:1, it is 5.0cSt linear dimethyl polysiloxanes then to add 25 DEG C of viscosity of 496.0g,
Carrier fluid content is 80%, opens mechanical agitation, is warming up to 80 DEG C, adds the vinyl complexing platinum catalyst of amount of calculation, makes
The content of metal platinum is 4.0ppm in system, and successive reaction 8.0h at such a temperature, the gel for then obtaining reaction pass through
The effect of colloid mill, a kind of translucent gel-thickened compound is obtained, be elastomer silicone polymer 8.
Embodiment 9
It is that 0.1%, 25 DEG C of viscosity is 50.0 cSt that 100.0g hydrogen contents are sequentially added in 1000mL four round flask
Hydrogen containing siloxane, 24.0g contents of ethylene is 0.5%, number-average molecular weight 10000, M/Q be 0.7 vinyl MQ silicon
Resin, both C=C/Si-H=1.2:1, it is 5.0cSt linear dimethyl polysiloxanes then to add 25 DEG C of viscosity of 496.0g,
Carrier fluid content is 80%, opens mechanical agitation, is warming up to 100 DEG C, adds the vinyl complexing platinum catalyst of amount of calculation,
The content for making metal platinum in system is 2.0ppm, and successive reaction 8.0h at such a temperature, the gel for then obtaining reaction pass through
The effect of colloid mill is crossed, obtains a kind of translucent gel-thickened compound, is elastomer silicone polymer 9.
Embodiment 10
It is that 0.2%, 25 DEG C of viscosity is 5.0 cSt that 25.0g hydrogen contents are sequentially added in 1000mL four round flask
Hydrogen containing siloxane, 5.0g contents of ethylene is 1.2%, number-average molecular weight 3000, and M/Q is 1.4 vinyl MQ silicon tree
Fat, both C=C/Si-H=1.2:1, it is 5.0cSt linear dimethyl polysiloxanes then to add 25 DEG C of viscosity of 570.0g, is carried
Body fluid content is 95%, opens mechanical agitation, is warming up to 80 DEG C, adds the vinyl complexing platinum catalyst of amount of calculation, makes body
The content of metal platinum is 10.0ppm in system, and successive reaction 0.5h at such a temperature, the gel for then obtaining reaction pass through
The effect of colloid mill, a kind of translucent gel-thickened compound is obtained, be elastomer silicone polymer 10.
Comparative example 1
With embodiment it is 2-in-1 into the object as a comparison of elastomer silicone polymer 2, use the hydrogeneous poly- silica of identical
Alkane, using the α that contents of ethylene is 0.3%, ω-bi-vinyl terminated polysiloxane, identical carrier fluid and content,
Conventional elastomers gel compound 11 is synthesized under identical reaction condition.
It is that 0.1%, 25 DEG C of viscosity is 50.0cSt that 100.0g hydrogen contents are sequentially added in 1000mL four round flask
Hydrogen containing siloxane, 33.3g contents of ethylene be 0.3% α, ω-bi-vinyl terminated polysiloxane, both C=C/
Si-H=1/1, then add 533.2g decamethylcyclopentaandoxanes (D5, 25 DEG C of viscosity are about 2.8cSt), carrier fluid content
For 80%, mechanical agitation is opened, 80 DEG C is warming up to, adds the isopropyl alcohol solution of chloroplatinic acid of amount of calculation, make metal platinum in system
Content is 3.0ppm, and successive reaction 8.0h at such a temperature, then will react obtained gel by three-roller type grinder
Effect, obtains a kind of translucent gel-thickened compound, is elastomer silicone polymer 11.
Comparative example 2
The object as a comparison of elastomer silicone polymer 9 synthesized with embodiment 9, uses the hydrogeneous poly- silica of identical
Alkane, using the α that contents of ethylene is 0.5%, ω-bi-vinyl terminated polysiloxane, identical carrier fluid and content,
Conventional elastomers gel compound 12 is synthesized under identical reaction condition.
It is that 0.1%, 25 DEG C of viscosity is 50.0cSt that 100.0g hydrogen contents are sequentially added in 1000mL four round flask
Hydrogen containing siloxane, 24.0g contents of ethylene be 0.5% α, ω-bi-vinyl terminated polysiloxane, both C=C/
Si-H=1.2:1, it is 5.0cSt linear dimethyl polysiloxanes then to add 25 DEG C of viscosity of 496.0g, and carrier fluid content is
80%, mechanical agitation is opened, is warming up to 100 DEG C, the vinyl complexing platinum catalyst of amount of calculation is added, makes metal platinum in system
Content be 2.0ppm, and the h of successive reaction 8.0 at such a temperature, then will react obtained gel and pass through the work of colloid mill
With obtaining a kind of translucent gel-thickened compound, be elastomer silicone polymer 12.
Cutaneous sense test comparison
Method of testing：0.5g elastomer silicone polymer is weighed, it is uniformly applied to the back of the hand that is clean, drying
Portion, identical size is sprawled into, the quality of its silty sense, the minimum ★ of silty sense score, highest are then judged by sense organ
For ★ ★ ★ ★ ★, select 10 veteran daily use chemicals formula engineers to carry out this evaluation, then integrate average, obtain
Point higher expression silty sense is better, and test result is shown in Table 1.
Table 1：Elastomer silicone polymer powder texture is tested
| Test sample title | Silty sense score |
| Elastomer silicone polymer 1 | ★★★★★ |
| Elastomer silicone polymer 2 | ★★★★ |
| Elastomer silicone polymer 3 | ★★★★★ |
| Elastomer silicone polymer 4 | ★★★★ |
| Elastomer silicone polymer 5 | ★★★ |
| Elastomer silicone polymer 6 | ★★★ |
| Elastomer silicone polymer 7 | ★★★★ |
| Elastomer silicone polymer 8 | ★★★★ |
| Elastomer silicone polymer 9 | ★★★★ |
| Elastomer silicone polymer 10 | ★★★ |
| Elastomer silicone polymer 11 | ★★ |
| Elastomer silicone polymer 12 | ★ |
It can be seen that by above-mentioned contrast test result, the score of elastomer silicone polymer 2 is far above elastomer polymer
11, the score of elastomer silicone polymer 9 is far above elastomer polymer 12, illustrates to synthesize based on Vinyl MQ silicon resin
The silty sense of elastomer polymer be much better than based on α, the elastomer polymer of ω-bi-vinyl terminated polysiloxane synthesis,
Skin sense with non-greasy.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, letter
Change, should be equivalent substitute mode, be included within protection scope of the present invention.
Claims (9)
1. a kind of elastomer silicone based on Vinyl MQ silicon resin, it is characterised in that polymerize to obtain by following component cross-link：
A) hydrogen containing siloxane；
B) Vinyl MQ silicon resin；
C) platinum catalyst；
D) carrier fluid.
A kind of 2. elastomer silicone based on Vinyl MQ silicon resin according to claim 1, it is characterised in that：It is described
Hydrogen containing siloxane is the dimethyl silicone polymer that side chain or end group contain Si -- H bond, and its H content is 0.05~0.5wt.%, its
Viscosity is 5.0~300.0cSt at 25 DEG C.
A kind of 3. elastomer silicone based on Vinyl MQ silicon resin according to claim 1, it is characterised in that：It is described
Vinyl MQ silicon resin, its contents of ethylene are 0.5~3.0wt.%, number-average molecular weight be 2000~10000, M/Q be 0.5~
1.5。
A kind of 4. elastomer silicone based on Vinyl MQ silicon resin according to claim 1, it is characterised in that：It is described
Platinum catalyst is the aqueous isopropanol or vinyl platinum complex of chloroplatinic acid.
A kind of 5. elastomer silicone based on Vinyl MQ silicon resin according to claim 1, it is characterised in that：It is described
Carrier fluid refers to the ring-type or linear polydimethylsiloxane- that viscosity is 1.0~50.0cSt at 25 DEG C, the content of carrier fluid
For 70~95wt.%.
6. a kind of preparation method of elastomer silicone based on Vinyl MQ silicon resin described in any one of Claims 1 to 5,
It is characterized in that including following preparation process：
50~100 DEG C are warming up to after hydrogen containing siloxane, Vinyl MQ silicon resin and carrier fluid are uniformly mixed, then
Platinum catalyst, 0.5~10.0h of insulation reaction are added, products therefrom obtains being based on vinyl MQ silicon after high speed shear acts on
The elastomer silicone of resin.
7. a kind of preparation method of elastomer silicone based on Vinyl MQ silicon resin according to claim 6, it is special
Sign is：The molar ratio of C=C keys and Si -- H bond in hydrogen containing siloxane is C=C/Si-H in the Vinyl MQ silicon resin
=(1~2)/1.
8. a kind of preparation method of elastomer silicone based on Vinyl MQ silicon resin according to claim 6, it is special
Sign is：The addition of the platinum catalyst is calculated with concentration of the metal platinum in system, concentration of the metal platinum in system
For 2~20ppm.
9. a kind of preparation method of elastomer silicone based on Vinyl MQ silicon resin according to claim 6, it is special
Sign is：The high speed shear effect refers to be handled using three-roller type grinder or colloid mill.
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| CN111217965A (en) * | 2020-02-24 | 2020-06-02 | 广东雷邦高新材料有限公司 | High-transparency high-refraction organic silicon elastomer gel and preparation method thereof |
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| CN112571907A (en) * | 2020-12-03 | 2021-03-30 | 安徽嘉明新材料科技有限公司 | TPU waterproof moisture permeable barrier film for medical protective clothing |
| CN112915046A (en) * | 2021-01-28 | 2021-06-08 | 广州市仲沅其新型材料有限公司 | Organic silicon elastomer gel and preparation method and application thereof |
| CN112915046B (en) * | 2021-01-28 | 2021-10-22 | 广州市仲沅其新型材料有限公司 | Organic silicon elastomer gel and preparation method and application thereof |
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