High-temperature-resistant combined antioxidant

Abstract

The invention relates to the technical field of antioxidants, and discloses a high-temperature-resistant combined antioxidant which comprises the following components in parts by weight: 20-30 parts of benzenediol; 15 to 25 parts of dodecanol; 8 to 12 parts of boron nitride; 12 to 20 parts of nano silicate; 3-6 parts of a catalyst; and 20-25 parts of a solvent. According to the high-temperature-resistant combined antioxidant, benzenediol and dodecanol serve as base materials to react, boron nitride and nano silicate are added, it can be guaranteed that the antioxidant forms a coating film on the surface of a product in the using process, gas is isolated, meanwhile, the high-temperature-resistant performance can be effectively improved, the antioxidant protection effect in the high-temperature environment is guaranteed, and the service life of the antioxidant is prolonged. The coating has the protection effects of oxidation resistance and corrosion resistance, and has a wide application prospect.

Description

Technical Field

[0001] The invention relates to the technical field of antioxidants, in particular to a high temperature resistant combined antioxidant. Background Art

[0002] Antioxidants are substances that prevent the adverse effects of oxygen. They can prevent or delay product oxidation, extend the life of products, and prevent product aging and corruption. In industry, antioxidants are usually added during product processing to improve the antioxidant effect of products. Commonly used antioxidants are antioxidants 1076 and 168.

[0003] However, when used in industries with higher operating temperatures, antioxidants 1076 and 168 have limited high-temperature antioxidant protection effects and poor stability, which can easily cause oxidation corrosion of the product, greatly reducing the product's service life. There are defects in the working range, which puts higher requirements on the high-temperature resistance of antioxidants.

[0004] In view of this, in-depth research was conducted on the above-mentioned problems, and a high-temperature resistant combined antioxidant was proposed. Summary of the invention

[0005] The object of the present invention is to provide a high temperature resistant combined antioxidant to solve the problem of limited high temperature resistance of existing antioxidants mentioned in the above background technology.

[0006] To achieve the above object, the present invention provides the following technical solution: a high temperature resistant combined antioxidant, comprising the following components in weight fractions:

[0007] 20-30 parts of hydroquinone;

[0008] 15-25 parts of dodecanol;

[0009] 8-12 parts of boron nitride;

[0010] 12-20 parts of nano silicate;

[0011] 3 to 6 parts of catalyst;

[0012] 20 to 25 parts of solvent.

[0013] As a preferred technical solution of the present invention, the molar ratio of dodecanol to hydroquinone is 1:1.1-1.5.

[0014] As a preferred technical solution of the present invention, the boron nitride is hexagonal boron nitride powder with a particle size of 5 to 10 um.

[0015] As a preferred technical solution of the present invention, the catalyst is one of concentrated sulfuric acid and phosphoric acid, and the solvent is ethanol.

[0016] A method for preparing a high temperature resistant combined antioxidant comprises the following steps:

[0017] Step 1: placing hydroquinone and a catalyst in a reaction vessel for heating and stirring for mixing reaction, and introducing an inert gas during the reaction;

[0018] Step 2: adding dodecanol into the reaction kettle in portions to participate in stirring and mixing reaction, and heating to obtain a mixture after the reaction;

[0019] Step 3: The obtained mixture is washed with deionized water to neutralize it, and then vacuum distilled to obtain a crystalline substance;

[0020] Step 4: Mix and dissolve the obtained crystals with a solvent, then centrifuge and filter, and dry to obtain a finished product.

[0021] As a preferred technical solution of the present invention, in the step 1, the heating temperature is controlled to 180-200° C., the stirring speed is 500-600 r / min, and the stirring time is 2-3 hours.

[0022] As a preferred technical solution of the present invention, the inert gas introduced in step 1 is nitrogen or argon.

[0023] As a preferred technical solution of the present invention, in the step 2, dodecanol is added to the reactor three times, and the addition of dodecanol is completed within two hours, with an interval of more than 30 minutes each time, and after the addition of dodecanol is completed, the temperature is raised to 220-240°C and stirred for 1.5-2 hours.

[0024] As a preferred technical solution of the present invention, in step three, reduced pressure distillation is carried out at a temperature of 120-140°C.

[0025] As a preferred technical solution of the present invention, in step 4, the drying temperature is controlled to be 110-120° C., and the drying time is 50-80 min.

[0026] Compared with the prior art, the beneficial effects of the present invention are: the high-temperature resistant combined antioxidant reacts with hydroquinone and dodecanol as the base material, and by adding boron nitride and nano-silicate, it can ensure that the antioxidant forms a coating film on the surface of the product during use to isolate the gas, and at the same time can effectively improve the high-temperature resistance performance, ensure the antioxidant protection effect in a high-temperature environment, have antioxidant and corrosion-resistant protection effects, and have broad application prospects. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 It is a schematic diagram of the main structure of the present invention. DETAILED DESCRIPTION

[0028] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0029] Embodiment 1

[0030] See also Figure 1 The technical solution of the present invention is: a high temperature resistant combined antioxidant, comprising the following components by weight:

[0031] Hydroquinone 20 parts;

[0032] 15 parts of dodecanol;

[0033] Boron nitride 8 parts;

[0034] 12 parts of nano silicate;

[0035] 3 parts of catalyst;

[0036] 20 parts of solvent.

[0037] The molar ratio of dodecanol to hydroquinone is 1:1.1.

[0038] The boron nitride is hexagonal boron nitride powder with a particle size of 5um.

[0039] The catalyst is one of concentrated sulfuric acid and phosphoric acid, and the solvent is ethanol.

[0040] A method for preparing a high temperature resistant combined antioxidant comprises the following steps:

[0041] Step 1: placing hydroquinone and a catalyst in a reaction vessel for heating and stirring for mixing reaction, and introducing an inert gas during the reaction;

[0042] Step 2: adding dodecanol into the reaction kettle in portions to participate in stirring and mixing reaction, and heating to obtain a mixture after the reaction;

[0043] Step 3: The obtained mixture is washed with deionized water to neutralize it, and then vacuum distilled to obtain a crystalline substance;

[0044] Step 4: Mix and dissolve the obtained crystals with a solvent, then centrifuge and filter, and dry to obtain a finished product.

[0045] In step 1, the heating temperature is controlled to 180° C., the stirring speed is 500 r / min, and the stirring time is 3 hours.

[0046] The inert gas introduced in step 1 is nitrogen or argon.

[0047] In step 2, dodecanol is added into the reactor in three times, and the addition of dodecanol is completed within two hours, with an interval of more than 30 minutes each time, and after the addition of dodecanol is completed, the temperature is raised to 220° C. and stirred for 2 hours.

[0048] Wherein in step 3, vacuum distillation is carried out at a temperature of 120°C.

[0049] In step 4, the drying temperature is controlled to be 110° C. and the drying time is controlled to be 80 min.

[0050] Embodiment 2

[0051] See also Figure 1 The technical solution of the present invention is: a high temperature resistant combined antioxidant, comprising the following components by weight:

[0052] Hydroquinone 20 parts;

[0053] 20 parts of dodecanol;

[0054] Boron nitride 8 parts;

[0055] 12 parts of nano silicate;

[0056] 4 parts of catalyst;

[0057] 20 parts of solvent.

[0058] The molar ratio of dodecanol to hydroquinone is 1:1.1.

[0059] The boron nitride is hexagonal boron nitride powder with a particle size of 6um.

[0060] The catalyst is one of concentrated sulfuric acid and phosphoric acid, and the solvent is ethanol.

[0061] A method for preparing a high temperature resistant combined antioxidant comprises the following steps:

[0062] Step 1: placing hydroquinone and a catalyst in a reaction vessel for heating and stirring for mixing reaction, and introducing an inert gas during the reaction;

[0063] Step 2: adding dodecanol into the reaction kettle in portions to participate in stirring and mixing reaction, and heating to obtain a mixture after the reaction;

[0064] Step 3: The obtained mixture is washed with deionized water to neutralize it, and then vacuum distilled to obtain a crystalline substance;

[0065] Step 4: Mix and dissolve the obtained crystals with a solvent, then centrifuge and filter, and dry to obtain a finished product.

[0066] In step 1, the heating temperature is controlled to 180° C., the stirring speed is 550 r / min, and the stirring time is 3 hours.

[0067] The inert gas introduced in step 1 is nitrogen or argon.

[0068] In step 2, dodecanol is added into the reactor in three times, and the addition of dodecanol is completed within two hours, with an interval of more than 30 minutes each time, and after the addition of dodecanol is completed, the temperature is raised to 220° C. and stirred for 2 hours.

[0069] Wherein in step 3, vacuum distillation is carried out at a temperature of 125°C.

[0070] In step 4, the drying temperature is controlled to be 110° C. and the drying time is controlled to be 70 min.

[0071] Embodiment 3

[0072] See also Figure 1 The technical solution of the present invention is: a high temperature resistant combined antioxidant, comprising the following components by weight:

[0073] Hydroquinone 25 parts;

[0074] 20 parts of dodecanol;

[0075] Boron nitride 10 parts;

[0076] 12 parts of nano silicate;

[0077] 4 parts of catalyst;

[0078] 22 parts of solvent.

[0079] The molar ratio of dodecanol to hydroquinone is 1:1.2.

[0080] The boron nitride is hexagonal boron nitride powder with a particle size of 6um.

[0081] The catalyst is one of concentrated sulfuric acid and phosphoric acid, and the solvent is ethanol.

[0082] A method for preparing a high temperature resistant combined antioxidant comprises the following steps:

[0083] Step 1: placing hydroquinone and a catalyst in a reaction vessel for heating and stirring for mixing reaction, and introducing an inert gas during the reaction;

[0084] Step 2: adding dodecanol into the reaction kettle in portions to participate in stirring and mixing reaction, and heating to obtain a mixture after the reaction;

[0085] Step 3: The obtained mixture is washed with deionized water to neutralize it, and then vacuum distilled to obtain a crystalline substance;

[0086] Step 4: Mix and dissolve the obtained crystals with a solvent, then centrifuge and filter, and dry to obtain a finished product.

[0087] In step 1, the heating temperature is controlled to 190° C., the stirring speed is 550 r / min, and the stirring time is 2.5 hours.

[0088] The inert gas introduced in step 1 is nitrogen or argon.

[0089] In step 2, dodecanol is added into the reactor in three times, and the addition of dodecanol is completed within two hours, with an interval of more than 30 minutes each time, and after the addition of dodecanol is completed, the temperature is raised to 230° C. and stirred for 2 hours.

[0090] Wherein in step 3, vacuum distillation is carried out at a temperature of 1230°C.

[0091] In step 4, the drying temperature is controlled to be 115° C. and the drying time is controlled to be 70 min.

[0092] Embodiment 4

[0093] See also Figure 1 The technical solution of the present invention is: a high temperature resistant combined antioxidant, comprising the following components by weight:

[0094] Hydroquinone 25 parts;

[0095] 25 parts of dodecanol;

[0096] Boron nitride 10 parts;

[0097] 15 parts of nano silicate;

[0098] 4 parts of catalyst;

[0099] 22 parts of solvent.

[0100] The molar ratio of dodecanol to hydroquinone is 1:1.2.

[0101] The boron nitride is hexagonal boron nitride powder with a particle size of 8um.

[0102] The catalyst is one of concentrated sulfuric acid and phosphoric acid, and the solvent is ethanol.

[0103] A method for preparing a high temperature resistant combined antioxidant comprises the following steps:

[0104] Step 1: placing hydroquinone and a catalyst in a reaction vessel for heating and stirring for mixing reaction, and introducing an inert gas during the reaction;

[0105] Step 2: adding dodecanol into the reaction kettle in portions to participate in stirring and mixing reaction, and heating to obtain a mixture after the reaction;

[0106] Step 3: The obtained mixture is washed with deionized water to neutralize it, and then vacuum distilled to obtain a crystalline substance;

[0107] Step 4: Mix and dissolve the obtained crystals with a solvent, then centrifuge and filter, and dry to obtain a finished product.

[0108] In step 1, the heating temperature is controlled to 1902° C., the stirring speed is 550 r / min, and the stirring time is 2.5 hours.

[0109] The inert gas introduced in step 1 is nitrogen or argon.

[0110] In step 2, dodecanol is added into the reactor in three times, and the addition of dodecanol is completed within two hours, with an interval of more than 30 minutes each time, and after the addition of dodecanol is completed, the temperature is raised to 230° C. and stirred for 2 hours.

[0111] Wherein in step 3, vacuum distillation is carried out at a temperature of 130°C.

[0112] In step 4, the drying temperature is controlled to be 115° C. and the drying time is controlled to be 65 min.

[0113] Embodiment 5

[0114] See also Figure 1 The technical solution of the present invention is: a high temperature resistant combined antioxidant, comprising the following components by weight:

[0115] Hydroquinone 28 parts;

[0116] 25 parts of dodecanol;

[0117] 1 part of boron nitride;

[0118] 20 parts of nano silicate;

[0119] 5 parts of catalyst;

[0120] 25 parts of solvent.

[0121] The molar ratio of dodecanol to hydroquinone is 1:1.4.

[0122] The boron nitride is hexagonal boron nitride powder with a particle size of 10um.

[0123] The catalyst is one of concentrated sulfuric acid and phosphoric acid, and the solvent is ethanol.

[0124] A method for preparing a high temperature resistant combined antioxidant comprises the following steps:

[0125] Step 1: placing hydroquinone and a catalyst in a reaction vessel for heating and stirring for mixing reaction, and introducing an inert gas during the reaction;

[0126] Step 2: adding dodecanol into the reaction kettle in portions to participate in stirring and mixing reaction, and heating to obtain a mixture after the reaction;

[0127] Step 3: The obtained mixture is washed with deionized water to neutralize it, and then vacuum distilled to obtain a crystalline substance;

[0128] Step 4: Mix and dissolve the obtained crystals with a solvent, then centrifuge and filter, and dry to obtain a finished product.

[0129] In step 1, the heating temperature is controlled to 200° C., the stirring speed is 600 r / min, and the stirring time is 2.5 hours.

[0130] The inert gas introduced in step 1 is nitrogen or argon.

[0131] In step 2, dodecanol is added into the reactor in three times, and the addition of dodecanol is completed within two hours, with an interval of more than 30 minutes each time, and after the addition of dodecanol is completed, the temperature is raised to 240° C. and stirred for 1.5 hours.

[0132] Wherein in step 3, vacuum distillation is carried out at a temperature of 140°C.

[0133] In step 4, the drying temperature is controlled to be 120° C. and the drying time is controlled to be 60 min.

[0134] Embodiment 6

[0135] See also Figure 1 The technical solution of the present invention is: a high temperature resistant combined antioxidant, comprising the following components by weight:

[0136] 30 parts of hydroquinone;

[0137] 25 parts of dodecanol;

[0138] Boron nitride 12 parts;

[0139] 20 parts of nano silicate;

[0140] 6 parts of catalyst;

[0141] 25 parts of solvent.

[0142] The molar ratio of dodecanol to hydroquinone is 1:1.5.

[0143] The boron nitride is hexagonal boron nitride powder with a particle size of 10um.

[0144] The catalyst is one of concentrated sulfuric acid and phosphoric acid, and the solvent is ethanol.

[0145] A method for preparing a high temperature resistant combined antioxidant comprises the following steps:

[0146] Step 1: placing hydroquinone and a catalyst in a reaction vessel for heating and stirring for mixing reaction, and introducing an inert gas during the reaction;

[0147] Step 2: adding dodecanol into the reaction kettle in portions to participate in stirring and mixing reaction, and heating to obtain a mixture after the reaction;

[0148] Step 3: The obtained mixture is washed with deionized water to neutralize it, and then vacuum distilled to obtain a crystalline substance;

[0149] Step 4: Mix and dissolve the obtained crystals with a solvent, then centrifuge and filter, and dry to obtain a finished product.

[0150] In step 1, the heating temperature is controlled to 200° C., the stirring speed is 600 r / min, and the stirring time is 2 hours.

[0151] The inert gas introduced in step 1 is nitrogen or argon.

[0152] In step 2, dodecanol is added into the reactor in three times, and the addition of dodecanol is completed within two hours, with an interval of more than 30 minutes each time, and after the addition of dodecanol is completed, the temperature is raised to 240° C. and stirred for 1.5 hours.

[0153] Wherein in step 3, vacuum distillation is carried out at a temperature of 140°C.

[0154] In step 4, the drying temperature is controlled to be 120° C. and the drying time is 50 min.

[0155] Comparative Example 1

[0156] The difference between this solution and Example 6 is that the other aspects are the same except that boron nitride is not added;

[0157] Comparative Example 2

[0158] The difference between this solution and Example 6 is that the nano-silicate is not added and the rest is the same;

[0159] Test: The antioxidants prepared in the above examples and comparative examples were applied to the surface of metal parts and tested at 1000°C. At the same time, a blank group was used to treat the test objects with antioxidant effects. The test results were analyzed as follows: Figure 1As shown in the figure, it can be seen that no oxidation phenomenon occurs in the embodiment, slight oxidation occurs in comparative example 1 after 36 hours, and slight oxidation occurs in comparative example 2 after 72 hours, indicating that the addition of boron nitride and nano-silicate has obvious anti-high temperature and anti-oxidation effects, and the anti-high temperature and anti-oxidation effects of boron nitride are more significant.

[0160] The contents not described in detail in this specification belong to the prior art known to professional and technical personnel in this field.

[0161] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A high temperature resistant combined antioxidant, characterized in that: The components include the following weight fractions: 20-30 parts of hydroquinone; 15-25 parts of dodecanol; 8-12 parts of boron nitride; 12-20 parts of nano silicate; 3 to 6 parts of catalyst; 20 to 25 parts of solvent.

2. A high temperature resistant combined antioxidant according to claim 1, characterized in that: The molar ratio of dodecanol to hydroquinone is 1:1.1-1.

5.

3. The high temperature resistant combined antioxidant according to claim 1, characterized in that: The boron nitride is hexagonal boron nitride powder with a particle size of 5 to 10 um.

4. The high temperature resistant combined antioxidant according to claim 1, characterized in that: The catalyst is one of concentrated sulfuric acid and phosphoric acid, and the solvent is ethanol.

5. A method for preparing a high temperature resistant combined antioxidant, characterized in that: The following steps are involved: Step 1: placing hydroquinone and a catalyst in a reaction vessel for heating and stirring for mixing reaction, and introducing an inert gas during the reaction; Step 2: adding dodecanol into the reaction kettle in portions to participate in stirring and mixing reaction, and heating to obtain a mixture after the reaction; Step 3: The obtained mixture is washed with deionized water to neutralize it, and then vacuum distilled to obtain a crystalline substance; Step 4: Mix and dissolve the obtained crystals with a solvent, then centrifuge and filter, and dry to obtain a finished product.

6. The method for preparing a high temperature resistant combined antioxidant according to claim 5, characterized in that: In the step 1, the heating temperature is controlled to 180-200° C., the stirring speed is 500-600 r / min, and the stirring time is 2-3 hours.

7. The method for preparing a high temperature resistant combined antioxidant according to claim 5, characterized in that: The inert gas introduced in step 1 is nitrogen or argon.

8. The method for preparing a high temperature resistant combined antioxidant according to claim 5, characterized in that: In the step 2, dodecanol is added into the reactor in three times, and the addition of dodecanol is completed within two hours, with an interval of more than 30 minutes each time, and after the addition of dodecanol is completed, the temperature is raised to 220-240° C. and stirred for 1.5-2 hours.

9. The method for preparing a high temperature resistant combined antioxidant according to claim 5, characterized in that: In the step 3, vacuum distillation is performed at a temperature of 120-140°C.

10. The method for preparing a high temperature resistant combined antioxidant according to claim 5, characterized in that: In the step 4, the drying temperature is controlled to be 110-120° C., and the drying time is 50-80 min.

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