CN107057114A - A kind of emulsion-type high dispersive antioxidant - Google Patents
A kind of emulsion-type high dispersive antioxidant Download PDFInfo
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- CN107057114A CN107057114A CN201710357727.9A CN201710357727A CN107057114A CN 107057114 A CN107057114 A CN 107057114A CN 201710357727 A CN201710357727 A CN 201710357727A CN 107057114 A CN107057114 A CN 107057114A
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- Prior art keywords
- paracresol
- toluene
- added
- emulsion
- antioxidant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/11—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by reactions increasing the number of carbon atoms
- C07C37/16—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by reactions increasing the number of carbon atoms by condensation involving hydroxy groups of phenols or alcohols or the ether or mineral ester group derived therefrom
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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Abstract
A kind of preparation method of emulsion-type polymolecularity antioxidant disclosed by the invention, comprises the following steps：Phenol and methanol are in catalyst Cs/SiO2The lower methylation reaction for carrying out phenol of effect, obtains product cresols；Toluene and complexing agent oxalic acid are added into reactor, cresols are added, by filtering, the paracresol oxalate complex of filtrate and white granular is obtained；Paracresol oxalate complex particle is added to the mixed solution of toluene and methanol, paracresol oxalate complex is filtrated to get；Obtained cresols oxalate complex is added to the water, isolated upper organic phase and lower floor's aqueous phase；Upper organic phase distillation removes solvent, obtains paracresol；The paracresol of gained is added in the Ludox that solid content is 40 50%, be stirred, gained emulsion-type high dispersive antioxidant.The emulsion-type high dispersive antioxidant dispersive property is good, and with excellent inoxidizability.
Description
Technical field
The present invention relates to technical field prepared by antioxidant, more particularly to a kind of emulsion-type high dispersive antioxidant.
Background technology
Rubber, plastics, latex etc. are as the important materials in daily life, and its application field is constantly widened, but macromolecule
Material is either natural or synthesis, all easily occurs oxidation reaction, makes material colour fading, yellowing, be cracked, tarnish.It is existing
There is the antioxidant bad dispersibility of technology, the application demand of be good at meeting rubber and plastics.Accordingly, it would be desirable to develop a emulsion-type
High dispersive antioxidant.
The content of the invention
It is an object of the invention to provide a kind of emulsion-type high dispersive antioxidant, one in above-mentioned prior art problem is solved
It is individual or multiple.
A kind of preparation method for emulsion-type polymolecularity antioxidant that the present invention is provided, comprises the following steps：
A1, phenol and methanol carry out the methylation reaction of phenol, the loading of the Cs under catalyst Cs/SiO2 effects
For 0.1%-2%, product cresols are obtained；
A2, addition toluene and complexing agent oxalic acid into reactor, the mass ratio of the toluene and oxalic acid is 1:1-1:3, lead to
Cross vapor and be heated to 90-110 DEG C, add the cresols, the mass ratio of the mixing phenol and toluene is 1:1-1:2,
1-2h is heated, by filtering, paracresol-oxalate complex of filtrate and white granular is obtained；
A3, the mixed solution by paracresol-oxalate complex particle addition toluene and methanol, the volume content of the methanol
For 20-40%, 1-2h is stirred, paracresol-oxalate complex is filtrated to get；
A4, cresols-oxalate complex that A3 is obtained is added to the water, is warming up to 40-60 DEG C, is incubated 1-2h, it is isolated
Upper organic phase and lower floor's aqueous phase；
A5, lower floor's aqueous phase are extracted by toluene, while toluene enters upper organic phase, described upper organic phase is distilled
Solvent is removed, described paracresol is obtained；
A6, the paracresol of gained is added in the Ludox that solid content is 40-50%, be stirred, described in gained
Emulsion-type high dispersive antioxidant.
In some embodiments, the preparation method of Ludox comprises the following steps：
B1, by weight/mass percentage composition be 10% sodium silicate solution, by cationic ion-exchange resin, obtain active silicic acid；
B2, by weight/mass percentage composition for 10% active silicic acid add retort, in retort add aqueous slkali regulation
PH value is 9-11, is heated by vapor, and heating and temperature control is at 100-120 DEG C, and the heat time is 10-20h, obtains solid content
For 43%-45%, particle diameter is 20-30nm silicon sol solution；
B3, by weight/mass percentage composition for 10% 20-30nm silicon sol solution add retort, in retort add
Aqueous slkali regulation pH value is 9-11, is heated by vapor, heating and temperature control is at 100-120 DEG C, and the heat time is 60-65h,
Solid content is obtained for 43%-45%, particle diameter is 100-120nm silicon sol solution.
In some embodiments, aqueous slkali is KOH, NaOH or TMAH.
Embodiment
The present invention is described in more detail below.
Case study on implementation 1：
A1, phenol and methanol are in catalyst Cs/SiO2The lower methylation reaction for carrying out phenol of effect, the loading of the Cs
For 0.1%, product cresols are obtained；
A2, addition toluene and complexing agent oxalic acid into reactor, the mass ratio of the toluene and oxalic acid is 1:1, pass through water
Steam is heated to 90 DEG C, adds the cresols, the mass ratio of the mixing phenol and toluene is 1:1,1h is heated, passes through mistake
Filter, obtains paracresol-oxalate complex of filtrate and white granular；
A3, the mixed solution by paracresol-oxalate complex particle addition toluene and methanol, the volume content of the methanol
For 20%, stirring 1h, paracresol-oxalate complex is filtrated to get；
A4, cresols-oxalate complex that a3 is obtained is added to the water, is warming up to 40 DEG C, is incubated 1h, isolated upper strata has
Machine phase and lower floor's aqueous phase；
A5, lower floor's aqueous phase are extracted by toluene, while toluene enters upper organic phase, described upper organic phase is distilled
Solvent is removed, described paracresol is obtained；
A6, by weight/mass percentage composition be 10% sodium silicate solution, by cationic ion-exchange resin, obtain active silicic acid；
A7, by weight/mass percentage composition for 10% active silicic acid add retort, in retort add KOH solution regulation
PH value is 9, is heated by vapor, and heating and temperature control is at 100 DEG C, and the heat time is 10h, and it is 43%% to obtain solid content,
Particle diameter is 20nm silicon sol solution；
A8, by weight/mass percentage composition for 10% 20nm silicon sol solution add retort, KOH is added in retort
Solution regulation pH value is 9, is heated by vapor, heating and temperature control is at 100 DEG C, and the heat time is 60h, obtains solid content and be
43%, particle diameter is 100nm silicon sol solution；
A9, the paracresol of gained is added in the Ludox that solid content is 40%, be stirred, the emulsion described in gained
Type high dispersive antioxidant.
Case study on implementation 2：
B1, phenol and methanol are in catalyst Cs/SiO2The lower methylation reaction for carrying out phenol of effect, the loading of the Cs
For 2%, product cresols are obtained；
B2, addition toluene and complexing agent oxalic acid into reactor, the mass ratio of the toluene and oxalic acid is 1:3, pass through water
Steam is heated to 110 DEG C, adds the cresols, the mass ratio of the mixing phenol and toluene is 1:2,2h is heated, is passed through
Filtering, obtains paracresol-oxalate complex of filtrate and white granular；
B3, the mixed solution by paracresol-oxalate complex particle addition toluene and methanol, the volume content of the methanol
For 40%, stirring 2h, paracresol-oxalate complex is filtrated to get；
B4, cresols-oxalate complex that b3 is obtained is added to the water, is warming up to 60 DEG C, is incubated 2h, isolated upper strata has
Machine phase and lower floor's aqueous phase；
B5, lower floor's aqueous phase are extracted by toluene, while toluene enters upper organic phase, described upper organic phase is distilled
Solvent is removed, described paracresol is obtained；
B6, by weight/mass percentage composition be 10% sodium silicate solution, by cationic ion-exchange resin, obtain active silicic acid；
B7, by weight/mass percentage composition for 10% active silicic acid add retort, in retort add NaOH solution adjust
It is 11 to save pH value, is heated by vapor, heating and temperature control is at 120 DEG C, and the heat time is 20h, and it is 45% to obtain solid content,
Particle diameter is 30nm silicon sol solution；
B8, by weight/mass percentage composition for 10% 30nm silicon sol solution add retort, in retort add
NaOH solution regulation pH value is 11, is heated by vapor, heating and temperature control is at 120 DEG C, and the heat time is 65h, consolidate
Content is 45%, and particle diameter is 120nm silicon sol solution；
B9, the paracresol of gained is added in the Ludox that solid content is 0%, be stirred, the emulsion described in gained
Type high dispersive antioxidant.
Case study on implementation 3：
C1, phenol and methanol are in catalyst Cs/SiO2The lower methylation reaction for carrying out phenol of effect, the loading of the Cs
For 1%, product cresols are obtained；
C2, addition toluene and complexing agent oxalic acid into reactor, the mass ratio of the toluene and oxalic acid is 1:2, pass through water
Steam is heated to 100 DEG C, adds the cresols, the mass ratio of the mixing phenol and toluene is 1:1.5, heating 1.5 is led to
Filtering, obtains paracresol-oxalate complex of filtrate and white granular；
C3, the mixed solution by paracresol-oxalate complex particle addition toluene and methanol, the volume content of the methanol
For 30%, stirring 1.5h, paracresol-oxalate complex is filtrated to get；
C4, cresols-oxalate complex that c3 is obtained is added to the water, is warming up to 5 DEG C, is incubated 1.5h, isolated upper strata
Organic phase and lower floor's aqueous phase；
C5, lower floor's aqueous phase are extracted by toluene, while toluene enters upper organic phase, described upper organic phase is distilled
Solvent is removed, described paracresol is obtained；
C6, by weight/mass percentage composition be 10% sodium silicate solution, by cationic ion-exchange resin, obtain active silicic acid；
C7, by weight/mass percentage composition for 10% active silicic acid add retort, in retort add tetramethyl hydrogen-oxygen
It is 10 to change ammonium salt solution regulation pH value, is heated by vapor, heating and temperature control is at 110 DEG C, and the heat time is 15h, consolidate
Content is 44%, and particle diameter is 25nm silicon sol solution；
C8, by weight/mass percentage composition for 10% 25nm silicon sol solution add retort, four are added in retort
Ammonium hydroxide solution regulation pH value is 10, is heated by vapor, and heating and temperature control is at 110 DEG C, and the heat time is
62h, it is 44% to obtain solid content, and particle diameter is 110nm silicon sol solution；
C9, the paracresol of gained is added in the Ludox that solid content is 45%, be stirred, the emulsion described in gained
Type high dispersive antioxidant.
Emulsion-type high dispersive antioxidant in the embodiment that the present invention is provided, its good dispersion, and antioxygenic property
It is excellent.
Presented above is only the preferred embodiment of the present invention, it is noted that to those skilled in the art, not
On the premise of departing from the invention design, various modifications and improvements can be made, these also should be regarded as the protection of the present invention
Within the scope of.
Claims (3)
1. a kind of preparation method of emulsion-type polymolecularity antioxidant, it is characterised in that comprise the following steps：
A1, phenol and methanol carry out the methylation reaction of phenol under catalyst Cs/SiO2 effects, and the loading of the Cs is
0.1%-2%, obtains product cresols；
A2, addition toluene and complexing agent oxalic acid into reactor, the mass ratio of the toluene and oxalic acid is 1:1-1:3, pass through water
Steam is heated to 90-110 DEG C, adds the cresols, the mass ratio of the mixing phenol and toluene is 1:1-1:2, heating
1-2h, by filtering, obtains paracresol-oxalate complex of filtrate and white granular；
A3, the mixed solution that paracresol-oxalate complex particle is added to toluene and methanol, the volume content of the methanol is
20-40%, stirs 1-2h, is filtrated to get paracresol-oxalate complex；
A4, cresols-oxalate complex that A3 is obtained is added to the water, is warming up to 40-60 DEG C, is incubated 1-2h, isolated upper strata
Organic phase and lower floor's aqueous phase；
A5, lower floor's aqueous phase are extracted by toluene, while toluene enters upper organic phase, described upper organic phase is distilled and removed
Solvent, obtains described paracresol；
A6, the paracresol of gained is added in the Ludox that solid content is 40-50%, be stirred, the emulsion described in gained
Type high dispersive antioxidant.
2. the preparation method of a kind of emulsion-type polymolecularity antioxidant according to claim 1, it is characterised in that described
The preparation method of Ludox comprises the following steps：
B1, by weight/mass percentage composition be 10% sodium silicate solution, by cationic ion-exchange resin, obtain active silicic acid；
B2, by weight/mass percentage composition for 10% active silicic acid add retort, in retort add aqueous slkali regulation pH value
For 9-11, heated by vapor, heating and temperature control is at 100-120 DEG C, and the heat time is 10-20h, obtain solid content and be
43%-45%, particle diameter is 20-30nm silicon sol solution；
B3, by weight/mass percentage composition for 10% 20-30nm silicon sol solution add retort, alkali soluble is added in retort
Liquid regulation pH value is 9-11, is heated by vapor, heating and temperature control is at 100-120 DEG C, and the heat time is 60-65h, is obtained
Solid content is 43%-45%, and particle diameter is 100-120nm silicon sol solution.
3. the preparation method of a kind of emulsion-type polymolecularity antioxidant according to claim 2, it is characterised in that described
Aqueous slkali be KOH, NaOH or TMAH.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710357727.9A CN107057114A (en) | 2017-05-19 | 2017-05-19 | A kind of emulsion-type high dispersive antioxidant |
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| CN201710357727.9A CN107057114A (en) | 2017-05-19 | 2017-05-19 | A kind of emulsion-type high dispersive antioxidant |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103145133A (en) * | 2013-03-17 | 2013-06-12 | 上虞市佳和化工有限公司 | Preparation method of silicon sol |
| CN103725051A (en) * | 2013-10-10 | 2014-04-16 | 弗克科技(苏州)有限公司 | Base material of inorganic coating and application of base material |
| CN103788476A (en) * | 2012-10-30 | 2014-05-14 | 中国石油化工股份有限公司 | Modified polypropylene resin and preparation method thereof |
| CN104058936A (en) * | 2014-06-20 | 2014-09-24 | 苏州飞翔新材料研究院有限公司 | Method for separation and purification of p-cresol |
-
2017
- 2017-05-19 CN CN201710357727.9A patent/CN107057114A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103788476A (en) * | 2012-10-30 | 2014-05-14 | 中国石油化工股份有限公司 | Modified polypropylene resin and preparation method thereof |
| CN103145133A (en) * | 2013-03-17 | 2013-06-12 | 上虞市佳和化工有限公司 | Preparation method of silicon sol |
| CN103725051A (en) * | 2013-10-10 | 2014-04-16 | 弗克科技(苏州)有限公司 | Base material of inorganic coating and application of base material |
| CN104058936A (en) * | 2014-06-20 | 2014-09-24 | 苏州飞翔新材料研究院有限公司 | Method for separation and purification of p-cresol |
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Application publication date: 20170818 |
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