CN111518393B - Silica gel sealing element and preparation method and application thereof - Google Patents
Silica gel sealing element and preparation method and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
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- B29B7/002—Methods
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/12—Materials for stopping leaks, e.g. in radiators, in tanks
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- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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Abstract
The invention discloses a silica gel sealing element which is prepared from the following raw materials in parts by weight: 80-100 parts of methyl vinyl phenyl silicone rubber, 5-8 parts of octamethylcyclotetrasilazane, 2-5 parts of hydrogen-containing silicone oil, 0.2-2.0 parts of accelerator TBzTDS, 0.5-1.0 part of vulcanizing agent BPDH, 3-5 parts of zinc oxide, 1-3 parts of zinc stearate, 0.5-1.5 parts of microcrystalline wax and 10-30 parts of fumed silica. The sealing gasket has good tolerance, effectively ensures the sealing performance, and has safe and stable product quality when in use. The invention also discloses a preparation method of the silica gel sealing element, which comprises the following steps: s1, mixing to obtain a rubber compound; s2, placing the rubber compound into a mold, and performing secondary vulcanization after primary vacuum vulcanization molding to obtain vulcanized rubber; s3, placing vulcanized rubber into a purifying solution, and soaking for 60-120 min at the temperature of 60-80 ℃, wherein the purifying solution comprises the following components in percentage by mass: 1-3 of absolute ethyl alcohol and pure water, and boiling the mixture in the pure water for 60-120 min. The invention also discloses application of the silica gel sealing piece in a wine container.
Description
Technical Field
The invention relates to the technical field of manufacturing of sealing elements, in particular to a silica gel sealing element and a preparation method and application thereof.
Background
After being brewed, the white spirit is generally stored in a storage container, and the storage time of the white spirit can be years or even decades, so that the sealing property for storing the white spirit products is highly required.
At present, the bottle mouth of the wine storage container is mostly sealed by a common silica gel sealing gasket, and due to the characteristics of wine, the common silica gel sealing element is in a high-acid, high-ester and high-ethanol environment for a long time, and can catalyze the common silica gel sealing element to separate out harmful substances to be mixed into the wine, so that the quality of the wine is influenced, and the health is harmed.
Disclosure of Invention
The invention aims to provide a silica gel sealing element, a preparation method and application thereof, which have good tolerance, effectively ensure the sealing performance and ensure the safe and stable product quality in use.
The silica gel sealing element is prepared from the following raw materials in parts by weight:
80-100 parts of methyl vinyl phenyl silicone rubber, 5-8 parts of octamethylcyclotetrasilazane, 2-5 parts of hydrogen-containing silicone oil, 0.2-2.0 parts of accelerator TBzTD0.5-1.0 parts of vulcanizing agent BPDH, 3-5 parts of zinc oxide, 1-3 parts of zinc stearate, 0.5-1.5 parts of microcrystalline wax and 10-30 parts of fumed silica.
A preparation method of a silica gel sealing element comprises the following steps:
s1, mixing, adjusting the temperature of a roller to be 50 ℃ or below, plasticating the methyl vinyl phenyl silicone rubber, after raw rubber is coated on the roller, sequentially adding octamethylcyclotetrasilazane, hydrogen-containing silicone oil, an accelerator TBztD, a vulcanizing agent BPDH, zinc oxide, zinc stearate, microcrystalline wax and fumed silica according to the parts by weight of the raw rubber in the claim 1, mixing to uniformly mix the components, passing through the mixture for 2-6 times, alternately rolling and triangular coating for multiple times, and then discharging the mixture to obtain the rubber compound.
And S2, vulcanizing, namely putting the rubber compound into a mold, and performing secondary vulcanization after primary vacuum vulcanization molding to obtain vulcanized rubber.
S3, performing purification treatment, namely placing vulcanized rubber in a purification solution, and soaking for 60-120 min at the temperature of 60-80 ℃, wherein the purification solution comprises the following components in a mass ratio of 6-8: 1-3 parts of absolute ethyl alcohol and pure water, and then boiling in the pure water for 60-120 min.
Further, the one-time vacuum vulcanization molding in S2 specifically includes: vulcanizing the rubber compound for 10-30 s under the condition that the vacuum degree is 20-30 inHg, and continuing vulcanizing after vacuumizing is stopped, wherein the total vulcanizing time is 150-300 s, and the vulcanizing temperature is 150-165 ℃. Through limiting the technological parameters of one-time vacuum vulcanization, the internal and external crosslinking degree of the product is uniform, the product performance is more stable, the phenomenon that the product is burnt outside and tender inside is avoided, slag chips are dropped outside the product in the using process, residual substances with incomplete vulcanization are released inside the product, and the performance stability of the product is further improved.
Further, the vulcanization temperature of the secondary vulcanization in the S2 is 180-240 ℃, and the vulcanization time is 2-4 h.
Furthermore, the conductivity of the pure water in the S3 is less than or equal to 5.0 mu S/cm, and the chemical purity of the pure water is limited, so that new impurities are prevented from being introduced into the product in the purification process, and the product quality is ensured.
Further, the mass ratio of the absolute ethyl alcohol to the pure water in the S3 is 7: 1.
further, the round rolls and the triangular bags are respectively rolled in the S1 for three times, so that the performance of the obtained product is ensured to be optimal.
The silica gel sealing piece or the silica gel sealing piece prepared by the preparation method is applied to an alcoholic liquor container.
Compared with the prior art, the invention has the following beneficial effects.
1. The silica gel sealing element has the advantages that the product performance and the raw material cost are comprehensively considered, the specific content of each raw material is limited, the silica gel sealing element is non-irritant and odorless, the chemical stability is good, and the silica gel sealing element can be safely and stably used in acid-base environments. And the working temperature range is wide, and the material can be used for a long time under the condition of-50-250 ℃. Meanwhile, the rubber has aging resistance, ozone resistance and saturated steam resistance, the compression deformation is less than 20 percent, and the rubber completely conforms to the regulation of GB4806.11-2016 (national food safety standard) rubber materials and products for food contact.
2. In the mixing process of the preparation method, the temperature of the roller is controlled to be 50 ℃ or below, so that the components and the crude rubber are uniformly mixed to the maximum extent, and the vulcanizing agent BPDH is prevented from being vulcanized and combusted in advance due to overhigh temperature, and the loss of the vulcanizing agent BPDH is avoided. Meanwhile, the temperature of the roller is low, so that the components are prevented from burning in the mixing process, the production risk is reduced, and the safe and high-quality mixing of the rubber material is realized.
3. The invention adopts secondary vulcanization, the rubber compound is vulcanized and molded under vacuum and vulcanization temperature during primary vulcanization, and mechanical opening and closing exhaust is cancelled, so that the scorching safety time of the product in the vulcanization process is more fully utilized, the stability of the product quality is ensured, and the safety and the cleanliness of product processing are improved. The secondary vulcanization ensures that the product is vulcanized more fully and has better performance, the residual non-body chemical substances in the product are promoted to be released, and the product quality is improved.
4. According to the preparation method, the acidic use environment of the product is simulated through the purifying liquid, the reaction of the product is catalyzed by the temperature which is more than twice of the temperature of the use environment, and the safety and reliability of the obtained silica gel sealing element in normal use are further ensured.
5. According to the invention, by combining specific raw material components and a preparation process, the prepared silica gel sealing element can be used for sealing the wine container, and the stability and safety of the silica gel sealing element in a high-acid, high-ester and high-ethanol environment for long-term use are ensured.
6. The invention has the advantages of easily obtained raw materials, simple process flow, stable product performance, safe and reliable use and suitability for large-scale industrial production.
Detailed Description
The present invention will be described in detail with reference to examples.
In a first embodiment, a method for manufacturing a silicone sealing member includes the following steps:
and S1, mixing, adjusting the temperature of the rollers to 45 ℃, adjusting the roller distance of the two rollers to 2.5mm, and putting 100 parts by weight of methyl vinyl phenyl silicone rubber between the two rollers for plastication to enable the raw rubber to wrap the rollers until the rubber wraps the rollers to form the adhesive tape with a smooth surface. After the raw rubber rolls are wrapped, adjusting the roll distance of the two rollers to 3mm, and allowing the raw rubber rolls to wrap to form a smooth adhesive tape, slowly adding an auxiliary agent, wherein the auxiliary agent comprises 2.5 parts by weight of octamethylcyclotetrasilazane, 1.5 parts by weight of hydrogen-containing silicone oil, 0.5 part by weight of promoter TBzTD, 0.25 part by weight of vulcanizing agent BPDH, 2 parts by weight of zinc oxide, 1 part by weight of zinc stearate, 0.5 part by weight of microcrystalline wax and 10 parts by weight of fumed silica, keeping a certain amount of accumulation rubber between the two rollers, and simultaneously carrying out left and right cutting knives. And after the additive is added for the first time, immediately cleaning the material tray to carry out the second feeding, wherein the addition amount of the second feeding is the same as that of the first feeding, and immediately cleaning the material tray to re-add the residual material between the two rollers after the feeding is finished each time. After all the raw materials are added, adjusting the roll distance of the two rollers to 2mm, performing thin-pass mixing for 2 times, alternately beating three round rolls and three triangular bags, and then discharging the sheets to obtain the rubber compound.
S2, vulcanizing, namely putting the rubber compound into a mold, feeding the mold into a vacuum vulcanization molding machine for primary vacuum vulcanization, vacuumizing to ensure that the vacuum degree of a working chamber of the vacuum vulcanization molding machine reaches 25inHg, vulcanizing the rubber compound for 20S under the condition that the vacuum degree is 25inHg, and continuing vulcanizing for 180S after vacuumizing is stopped, wherein the vulcanizing temperature is 160 ℃.
And immediately sending the product into a special precise forced convection rolling oven for secondary vulcanization after the primary vacuum vulcanization is finished, wherein the vulcanization temperature is 200 ℃, and the vulcanization time is 3 hours, so as to obtain the vulcanized rubber.
S3, purifying, namely, placing vulcanized rubber into a purifying solution and soaking for 90min at the temperature of 70 ℃, wherein the purifying solution comprises the following components in mass ratio of 7: 1 and then boiling in pure water for 90min to obtain the silica gel sealing piece. The purity of the absolute ethyl alcohol is 99.9%, the conductivity of pure water is less than or equal to 5.0 mu S/cm, and by limiting the chemical purity of the absolute ethyl alcohol and the pure water, the introduction of new impurities into the product in the purification process is avoided, and the product quality is ensured.
And (3) carrying out performance detection on the obtained silica gel sealing element, wherein the performance detection specifically comprises the following steps: the plasticizer content and the plasticizer migration amount are measured according to GB31604.30-2016, sensory measurement is carried out according to GB4806.11-2016, the total migration amount is measured according to GB31604.8-2016, the potassium permanganate consumption is measured according to GB31604.2-2016, and heavy metal is measured according to GB 31604.9-2016. Wherein, the simulators selected during the total migration measurement are an acetic acid solution with the volume fraction of 4% and an ethanol solution with the volume fraction of 60%, the migration test time is 10d, and the migration test temperature is 40 ℃.
The test results are shown in tables 1 and 2.
TABLE 1 measurement of plasticizer content
| Serial number | Name of plasticizer | Determination of the Condition |
| 1 | Dimethyl phthalate (DMP) | Not detected out |
| 2 | Phthalic acid Diethyl Ester (DEP) | Undetected |
| 3 | Diallyl phthalate (DAP) | Undetected |
| 4 | Diisobutyl phthalate (DIBP) | Not detected out |
| 5 | Dibutyl phthalate (DBP) | Not detected out |
| 6 | Bis (2-methoxy) ethyl phthalate (DMEP) | Not detected out |
| 7 | Bis (4-methyl-2-pentyl) phthalate (BMPP) | Undetected |
| 8 | Bis (2-ethoxy) ethyl phthalate (DEEP) | Not detected out |
| 9 | Diamyl phthalate (DPP) | Not detected out |
| 10 | Dihexyl phthalate (DHXP) | Not detected out |
| 11 | Butyl Benzyl Phthalate (BBP) | Undetected |
| 12 | Bis (2-butoxy) ethyl phthalate (DBEP) | Not detected out |
| 13 | Dicyclohexyl phthalate (DCHP) | Not detected out |
| 14 | Di (2-ethyl) hexyl phthalate (DEHP) | Undetected |
| 15 | Diphenyl phthalate (DPhP) | Not detected out |
| 16 | Di-n-octyl phthalate (DNOP) | Not detected out |
| 17 | Diisononyl phthalate (DINP) | Undetected |
| 18 | Dinonyl phthalate (DNP) | Not detected out |
TABLE 2 hygiene index test results
As can be seen from tables 1 and 2, the silica gel sealing member obtained by combining the raw materials in the above proportions and a specific preparation process completely meets the specification of GB4806.11-2016 (national food safety standard rubber material and product for food contact), can be used for sealing containers for alcoholic beverages, and ensures the stability and safety of the silica gel sealing member in long-term use in high-acid, high-ester, and high-ethanol environments. And the adopted raw materials are easy to obtain, the process flow is simple, the product performance is stable, the use is safe and reliable, and the method is suitable for large-scale industrial production.
Embodiment two, a silica gel sealing member is prepared from the following raw materials in parts by weight: 100 parts of methyl vinyl phenyl silicone rubber, 8 parts of octamethylcyclotetrasilazane, 5 parts of hydrogen-containing silicone oil, 0.2 part of accelerator TBzTD, 1.0 part of vulcanizing agent BPDH, 3 parts of zinc oxide, 1 part of zinc stearate, 0.5 part of microcrystalline wax and 10 parts of fumed silica.
The preparation method of the silica gel sealing piece comprises the following steps:
and S1, mixing, adjusting the temperature of the rollers to 50 ℃, adjusting the roller distance of the two rollers to 3.0mm, and putting 100 parts by weight of methyl vinyl phenyl silicone rubber between the two rollers for plastication to enable the raw rubber to wrap the rollers until the rubber wraps the rollers to form the adhesive tape with a smooth surface. After the raw rubber is coated on the roller, the roller distance between the two rollers is adjusted to 3.5mm, and the auxiliary agent is slowly added when the raw rubber is coated on the roller to form a smooth adhesive tape. After all the raw materials are added, adjusting the roll distance of the two rollers to 2.5mm, mixing twice through thin-pass, alternately beating three round rolls and three triangular bags, and then discharging the sheets to obtain the rubber compound.
S2, vulcanizing, namely putting the rubber compound into a mold, feeding the mold into a vacuum vulcanization molding machine for primary vacuum vulcanization, vacuumizing to ensure that the vacuum degree of a working chamber of the vacuum vulcanization molding machine reaches 20inHg, vulcanizing the rubber compound for 10S under the condition that the vacuum degree is 20inHg, stopping vacuumizing, and continuing vulcanizing for 140S at the vulcanization temperature of 165 ℃.
And immediately sending the product into a special precise forced convection rolling oven for secondary vulcanization after the primary vacuum vulcanization is finished, wherein the vulcanization temperature is 180 ℃, and the vulcanization time is 4 hours, so as to obtain the vulcanized rubber.
S3, performing purification treatment, namely placing vulcanized rubber in a purification solution and soaking for 90min at the temperature of 70 ℃, wherein the purification solution comprises the following components in a mass ratio of 7: 1, boiling in pure water for 90min to obtain a silica gel sealing element, wherein the silica gel sealing element completely accords with the regulation of GB4806.11-2016 (national food safety standard) rubber material and product for food contact.
In the third embodiment, a silica gel sealing member is prepared from the following raw materials in parts by weight: 80 parts of methyl vinyl phenyl silicone rubber, 5 parts of octamethylcyclotetrasilazane, 4 parts of hydrogen-containing silicone oil, 1.5 parts of accelerator TBzTD, 0.8 part of vulcanizing agent BPDH, 5 parts of zinc oxide, 2 parts of zinc stearate, 1.2 parts of microcrystalline wax and 25 parts of fumed silica.
The preparation method of the silica gel sealing piece comprises the following steps:
s1, mixing, adjusting the temperature of the rollers to 50 ℃, adjusting the roller distance of the two rollers to 3.0mm, putting 100 parts by weight of methyl vinyl phenyl silicone rubber between the two rollers for plastication, and allowing the raw rubber to wrap the rollers until the rubber wraps the rollers to form the adhesive tape with a smooth surface. After the raw rubber is coated on the roller, the roller distance between the two rollers is adjusted to 3.5mm, and the auxiliary agent is slowly added when the raw rubber is coated on the roller to form a smooth adhesive tape. After all the raw materials are added, adjusting the roll distance of the two rollers to 2.5mm, mixing twice through thin-pass, alternately beating three round rolls and three triangular bags, and then discharging the sheets to obtain the rubber compound.
S2, vulcanizing, namely putting the rubber compound into a mold, feeding the mold into a vacuum vulcanization molding machine for primary vacuum vulcanization, vacuumizing to ensure that the vacuum degree of a working chamber of the vacuum vulcanization molding machine reaches 30inHg, maintaining the rubber compound to be vulcanized for 25S under the condition that the vacuum degree is 30inHg, stopping vacuumizing, and continuing to vulcanize for 150S at the vulcanization temperature of 155 ℃.
And immediately sending the product into a special precise forced convection rolling oven for secondary vulcanization after the primary vacuum vulcanization is finished, wherein the vulcanization temperature is 240 ℃, and the vulcanization time is 2 hours, so as to obtain the vulcanized rubber.
S3, purifying, namely, placing vulcanized rubber into a purifying solution and soaking for 60min at the temperature of 80 ℃, wherein the purifying solution comprises the following components in percentage by mass: 1, boiling in pure water for 90min to obtain a silica gel sealing element, wherein the silica gel sealing element completely accords with the regulation of GB4806.11-2016 (national food safety standard) rubber material and product for food contact.
In the fourth embodiment, different vulcanizing agents are used for comparative analysis, the silica gel sealing element described in the first embodiment is used as a test group, the types of the vulcanizing agents are changed, the contents of other components are controlled to be the same, a vulcanizing agent DTBP is used as a first control group, a DTBP/bis-penta composite vulcanizing agent is used as a second control group, a bis-penta vulcanizing agent is used as a third control group, the product is prepared by a preparation method with the same process parameters, and mass spectrometry is respectively performed on the products of the test group, the first control group, the second control group and the third control group according to GB 8112 plus 2011-T determination of residual quantity of volatile methyl cyclosiloxane in silicone rubber, and the results are shown in fig. 1 to 4.
As can be seen from fig. 1 to 4, the amount of the residues precipitated in the first control group, the second control group and the third control group is much higher than that in the test group, and when the residues are first measured in the test group, the relative abundance value corresponding to each residue is low, and the amount of the residues precipitated on the surface is very small and almost negligible. The method has the advantages that the testing time of the test group is prolonged, the subsequent substance residues are still less in precipitation amount, the performance of the silica gel sealing element is directly influenced by the selection of the vulcanizing agent, and the obtained silica gel sealing element is free from irritation and odor, good in chemical stability and capable of being safely and stably used in acid-base environments by selecting the specific vulcanizing agent and combining the limitation of the contents of other components. And the working temperature range is wide, and the material can be used for a long time under the condition of-50-250 ℃. Meanwhile, the rubber has aging resistance, ozone resistance and saturated steam resistance, the compression deformation is less than 20 percent, and the rubber completely conforms to the regulation of GB4806.11-2016 (national food safety standard) rubber materials and products for food contact.
The above description is only a preferred embodiment of the present application and should not be taken as limiting the present application, and any modifications, equivalents, improvements, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (7)
1. The silica gel sealing element is characterized by being prepared from the following raw materials in parts by weight:
80-100 parts of methyl vinyl phenyl silicone rubber, 5-8 parts of octamethylcyclotetrasilazane, 2-5 parts of hydrogen-containing silicone oil, 0.2-2.0 parts of accelerator TBzTDS, 0.5-1.0 part of vulcanizing agent BPDH, 3-5 parts of zinc oxide, 1-3 parts of zinc stearate, 0.5-1.5 parts of microcrystalline wax and 10-30 parts of fumed silica;
the preparation method of the silica gel sealing piece comprises the following steps:
s1, mixing, adjusting the temperature of a roller to be 50 ℃ or below, plasticating methyl vinyl phenyl silicone rubber, after raw rubber is coated on the roller, sequentially adding octamethylcyclotetrasilazane, hydrogen-containing silicone oil, an accelerator TBzTD, a vulcanizing agent BPDH, zinc oxide, zinc stearate, microcrystalline wax and gas phase method white carbon black according to the weight parts, mixing to uniformly mix the components, performing thin passing for 2-6 times, alternately rolling and triangular wrapping for multiple times, and then discharging to obtain mixed rubber;
s2, vulcanizing, namely putting the rubber compound into a mold, and performing secondary vulcanization after primary vacuum vulcanization molding to obtain vulcanized rubber;
s3, purifying, namely placing vulcanized rubber into a purifying solution and soaking for 60-120 min at the temperature of 60-80 ℃, wherein the purifying solution comprises the following components in parts by mass: 1-3 parts of absolute ethyl alcohol and pure water, and then boiling in the pure water for 60-120 min.
2. The silicone rubber seal according to claim 1, wherein the one-time vacuum vulcanization molding in S2 is specifically: vulcanizing the rubber compound for 10-30 s under the condition that the vacuum degree is 20-30 inHg, and continuing vulcanizing after vacuumizing is stopped, wherein the total vulcanizing time is 150-300 s, and the vulcanizing temperature is 150-165 ℃.
3. The silicone seal according to claim 1 or 2, characterized in that: and the vulcanization temperature of the secondary vulcanization in the S2 is 180-240 ℃, and the vulcanization time is 2-4 h.
4. The silicone seal according to claim 1 or 2, characterized in that: the conductivity of the pure water in the S3 is less than or equal to 5.0 mu S/cm.
5. The silicone seal according to claim 1 or 2, characterized in that: the mass ratio of the absolute ethyl alcohol to the pure water in the S3 is 7: 1.
6. the silicone seal according to claim 1 or 2, characterized in that: and (5) respectively rolling and triangular wrapping three times in the S1.
7. Use of the silica gel sealing member according to any one of claims 1 to 6 in an alcoholic beverage container.
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