WO2017024608A1 - 一种尼龙耐候助剂的制备方法 - Google Patents

一种尼龙耐候助剂的制备方法 Download PDF

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WO2017024608A1
WO2017024608A1 PCT/CN2015/087650 CN2015087650W WO2017024608A1 WO 2017024608 A1 WO2017024608 A1 WO 2017024608A1 CN 2015087650 W CN2015087650 W CN 2015087650W WO 2017024608 A1 WO2017024608 A1 WO 2017024608A1
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tetramethyl
preparation
nylon
aminopiperidine
isophthalate
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PCT/CN2015/087650
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English (en)
French (fr)
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陆园
蔡智奇
余小红
王轲
程江
文秀芳
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新秀化学（烟台）有限公司
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D211/00—Heterocyclic compounds containing hydrogenated pyridine rings, not condensed with other rings
    • C07D211/04—Heterocyclic compounds containing hydrogenated pyridine rings, not condensed with other rings with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
    • C07D211/06—Heterocyclic compounds containing hydrogenated pyridine rings, not condensed with other rings with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members
    • C07D211/36—Heterocyclic compounds containing hydrogenated pyridine rings, not condensed with other rings with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
    • C07D211/56—Nitrogen atoms
    • C07D211/58—Nitrogen atoms attached in position 4

Definitions

  • the invention relates to the field of chemical industry, in particular to a preparation method of a nylon weathering aid.
  • Nylon (PA) is a crystalline thermoplastic engineering plastic with many excellent properties such as high tensile strength and good wear resistance. It is widely used. However, due to the amide group (-NHCO-) contained in the nylon structure, it belongs to the chromophore group and has a strong polarity. It is a weak link of the entire chain and is susceptible to environmental factors such as heat, oxygen, ultraviolet rays and moisture. Affects, a series of pyrolysis reactions occur, producing water, CO 2 , CO, hydrocarbons and a small amount of cyclopentanone, which causes the polymer backbone to be cut, the color of the polymer changes, and various properties are degraded.
  • amide group -NHCO-
  • nylon auxiliary agent light stabilizer, antioxidant, weathering aid
  • Weathering aid N,N-bis(2,2,6,6-tetramethyl-4-piperidyl)-1,3-phthalamide has excellent light stability effect on nylon products and added value High, application prospects, and its quality has a great impact on the anti-aging properties of nylon polymerization, spinning or products, specifically, N, N-di (2,2,6,6-tetramethyl
  • the structure of 4-piperidinyl)-1,3-phthalamide is as follows:
  • the patent ZL 201310110901.1 reports the synthesis method of the above nylon auxiliary agent: using 2,2,6,6-tetramethyl-4-aminopiperidine and isophthalic acid chloride as raw materials, in anhydrous organic
  • the reaction is carried out in a solvent at -5 to 25 ° C, and the reaction is completed until the precipitation is complete.
  • the liquid is filtered, the filter cake is washed with anhydrous organic solvent, and then dried to obtain an intermediate; the intermediate and water are uniformly stirred at room temperature, neutralized with sodium hydroxide solution, filtered, washed with water, and the filter cake is dried.
  • the target product is obtained afterwards.
  • the reactant contains an acid chloride, and the raw material II is easily hydrolyzed.
  • the excess II In order to increase the yield, an excess of the raw material II is required, but the excess II needs to be washed out with an excess of water, which generates a large amount of waste water, and the yield is relatively high. Low, resulting in its inability to industrialize mass production.
  • the object of the present invention is to provide a preparation method of a nylon weathering aid N,N-bis(2,2,6,6-tetramethyl-4-piperidyl)-1,3-phthalic acid amide.
  • a preparation method of N,N-bis(2,2,6,6-tetramethyl-4-piperidyl)-1,3-phthalic acid amide comprising the following steps: in a solvent, 2 Using 2,6,6-tetramethyl-4-aminopiperidine and dialkyl isophthalate as raw materials, the aminolysis of the ester is carried out under the catalysis of the catalyst to obtain N,N-di(2,2,6). , 6-tetramethyl-4-piperidinyl)-1,3-phthalic acid amide.
  • the technical solution of the present invention includes the following steps:
  • the reaction time of the step (1) is 20 to 24 hours, preferably 24 hours.
  • Step (1) generally requires stirring for 1 to 5 minutes.
  • the dialkyl isophthalate in the step (1) is one or two selected from the group consisting of dimethyl isophthalate or diethyl isophthalate.
  • the molar ratio of the 2,2,6,6-tetramethyl-4-aminopiperidine to the dialkyl isophthalate is from 2.4:1 to 3.3:1, preferably 2.9:1.
  • the solvent is one selected from the group consisting of toluene, methanol or ethanol. Specifically, the mass ratio of 2,2,6,6-tetramethyl-4-aminopiperidine to the solvent is 1:7 to 1:10, At this time, the dissolved and stirred state of the reactants is the best.
  • the catalyst is selected from one or more of trimethyl aluminum, diethyl aluminum, tripropyl aluminum, tributyl aluminum or triisopropyl aluminum, preferably It is trimethyl aluminum. More specifically, the catalyst comprises from 0.5 to 3% by weight of the total mass of the reactant (2,2,6,6-tetramethyl-4-aminopiperidine, dialkyl isophthalate and solvent).
  • the filtrate obtained in the step (2) contains a catalyst and an excess of 2,2,6,6-tetramethyl-4-aminopiperidine in addition to the solvent, so the step (2) is obtained.
  • the filtrate can be applied as a reaction solvent of the step (1) in the next reaction, that is, the filtrate obtained in the step (2) is reused as a solvent in the next step (1).
  • the molar ratio of the 2,2,6,6-tetramethyl-4-aminopiperidine to the dialkyl isophthalate is 2.0:1 to 2.3: 1, preferably 2.23:1.
  • the invention uses 2,2,6,6-tetramethyl-4-aminopiperidine and dialkyl isophthalate as raw materials to obtain N,N-bis (2,2,6,6 by aminolysis reaction).
  • -tetramethyl-4-piperidinyl)-1,3-phthalic acid amide avoiding the use of acid chlorides to participate in the reaction, without NaOH neutralization, without the need to treat chlorine-containing wastewater, and the later sewage treatment is relatively easy and relatively environmentally friendly;
  • the filtrate produced in the reaction can be applied, which reduces the industrial production cost.
  • the preparation method of the invention has the advantages of simple process and high utilization rate of raw materials, and N, N-di (2, prepared by the method of the invention) 2,6,6-Tetramethyl-4-piperidinyl)-1,3-phthalic acid amide has the advantages of good product quality and no residual chlorine ions.
  • This embodiment is a preparation method of N,N-bis(2,2,6,6-tetramethyl-4-piperidyl)-1,3-phthalamide, and specifically comprises the following steps:
  • the above washing is carried out with water, specifically: washing with deionized water for 3 to 5 times.
  • the above filtration was dried, specifically: drying at 80 ° C for 12 h.
  • This embodiment is a preparation method of N,N-bis(2,2,6,6-tetramethyl-4-piperidyl)-1,3-phthalamide, and specifically comprises the following steps:
  • This embodiment is a preparation method of N,N-bis(2,2,6,6-tetramethyl-4-piperidyl)-1,3-phthalamide, and specifically comprises the following steps:
  • This embodiment is a preparation method of N,N-bis(2,2,6,6-tetramethyl-4-piperidyl)-1,3-phthalamide, and specifically comprises the following steps:
  • This embodiment is a preparation method of N,N-bis(2,2,6,6-tetramethyl-4-piperidyl)-1,3-phthalamide, and specifically comprises the following steps:
  • This embodiment differs from the first embodiment only in that the amount of dimethyl phthalate added in step (1) is different.
  • the amount of dimethyl phthalate added is 4.46 g. (about 0.023 mol).
  • N,N-bis(2,2,6,6-tetramethyl-4-piperidyl)-1,3-phthalic acid amide was 80%, the melting point was 272.2 ° C, and the content was 98.87%. HPLC).
  • This embodiment differs from Example 1 only in that the amount of dimethyl phthalate added in step (1) is different.
  • the amount of dimethyl phthalate added is 6.15 g (about 0.032 mol). ).
  • This embodiment differs from Example 5 only in that step (1) the amount of dimethyl phthalate added is different.
  • the amount of dimethyl phthalate added is 5.63 g (about 0.029 mol). ).
  • N,N-bis(2,2,6,6-tetramethyl-4-piperidyl)-1,3-phthalic acid amide was 80%, the melting point was 272.2 ° C, and the content was 98.68%. HPLC).
  • This embodiment differs from Example 5 only in that the amount of dimethyl phthalate added in step (1) is different.
  • the amount of dimethyl phthalate added is 4.82 g (about 0.025 mol). .
  • Comparative Example 1 differs from the examples only in that no catalyst was added in Comparative Example 1, and the remaining steps were the same, and N,N-bis(2,2,6,6-tetramethyl-4-piperidine was not finally obtained.
  • Base - 1,3-phthalamide.
  • Comparative Example 2 differs from the examples only in that, in Comparative Example 2, ammonium chloride was used as a catalyst. The remaining steps were the same, and N,N-bis(2,2,6,6-tetramethyl-4-piperidyl)-1,3-phthalamide was not finally obtained.

Abstract

本发明公开了一种尼龙耐候助剂的制备方法，具体包括以下步骤：在溶剂中，以2,2,6,6-四甲基-4-氨基哌啶和间苯二甲酸二烷基酯为原料，在催化剂的催化下发生酯的氨解反应得到尼龙耐候助剂N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺。本发明避免了采用酰氯参与反应，无需NaOH中和，无需处理含氯废水，后期污水处理相对容易，相对环境友好；而且过滤后的滤液可套用参与下一次反应，降低了工业化生产成本。

Description

一种尼龙耐候助剂的制备方法 技术领域
本发明涉及化工领域，特别涉及一种尼龙耐候助剂的制备方法。
背景技术
尼龙(PA)是一种结晶性热塑性工程塑料，具有拉伸强度高、耐磨性能好等许多优异性能，用途十分广泛。但由于尼龙结构中含有的酰胺基团(-NHCO-)，其属于生色基团，具有较强的极性，是整个链的薄弱环节，容易受到热、氧、紫外线、水分等环境因素的影响，发生一系列的热解反应，生成水、CO2、CO、烃与少量环戊酮，从而导致聚合物主链被切断，使聚合物的颜色发生变化，各项性能下降。因此需要通过在尼龙聚合，尼龙纺丝或改性制品中通过添加尼龙助剂(光稳定剂、抗氧剂、耐候助剂)来提高尼龙的耐候性，尽可能地保持制品长期使用后的外观和颜色，延长其使用寿命。
耐候助剂N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺对尼龙制品具有极好的光稳定效果，产品附加价值高、应用前景大，而且其品质的好坏对尼龙聚合、纺丝或制品的抗老化性能具有很大的影响，具体的，N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺的结构如下所示：
Figure PCTCN2015087650-appb-000001
传统合成方法中，例如专利ZL 201310110901.1报道了上述尼龙助剂的合成方法：以2,2,6,6-四甲基-4-氨基哌啶和间苯二甲酸酰氯为原料，在无水有机溶剂中于-5～25℃进行反应，反应至沉淀完全，反应 液经过滤，滤饼经无水有机溶剂洗涤后，烘干得中间体；在室温下将中间体与水搅拌均匀后，用氢氧化钠溶液中和，过滤，用水洗涤，滤饼经烘干后得到目标产物。
Figure PCTCN2015087650-appb-000002
上述制备尼龙助剂的方法的主要缺点为：1、需NaOH中和；2、需后期污水处理；3、含酰氯参与反应。
又如专利WO/9743335中报道的尼龙助剂N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺的合成路线如下所示：
Figure PCTCN2015087650-appb-000003
在上述合成方法中反应物中含有酰氯，且原料II易水解，为了提高产率，需要原料II过量，但是过量的II需要使用过量的水冲洗除净，会产生大量废水，且产率相对较低，导致其不能工业化大量生产。
再如专利US/20060199963中N,N-二(2,2,6,6-四甲基-4-哌啶 基)-1,3-苯二甲酰胺的合成路线如下所示：
Figure PCTCN2015087650-appb-000004
另外，专利WO/2004016591中N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺的合成路线如下所示：
Figure PCTCN2015087650-appb-000005
由上述合成路线可以看出，因为酰氯活性高，在现有的N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺的制备方法中，反应原料中均含有酰氯，但是以酰氯作为反应原料，会对后续处理带来很大麻烦，目标产品中未除净的氯离子对产品品质的好坏有很大影响。因此，亟须研发一种以酰氯之外的其他原料合成N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺的方法。
发明内容
本发明的目的是提供一种尼龙耐候助剂N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺的制备方法。
为达到上述目的，具体采用如下的技术方案：
一种N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺的制备方法，包括以下步骤：在溶剂中，以2,2,6,6-四甲基-4-氨基哌啶和间苯二甲酸二烷基酯为原料，在催化剂的催化下发生酯的氨解反应得到N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺。
在本发明的技术方案中，反应原料2,2,6,6-四甲基-4-氨基哌啶和间苯二甲酸二烷基酯均可采用市售的所有产品。
具体的，本发明的技术方案包括以下步骤：
(1)将2,2,6,6-四甲基-4-氨基哌啶溶于溶剂中，加入催化剂，充分搅拌，再加入间苯二甲酸二烷基酯，40～80℃条件下反应，得到混合液；
(2)将步骤(1)得到的混合液经冷却、过滤后分别得到滤液和固体物质，固体物质经水洗干燥后即得N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺。
本发明的技术方案可以用以下的反应历程所表示：
Figure PCTCN2015087650-appb-000006
在本发明的技术方案中，步骤(1)的反应时间为20～24h，优选为24h。步骤(1)一般需要搅拌1～5min。
具体的，步骤(1)中所述间苯二甲酸二烷基酯选自间苯二甲酸二甲酯或间苯二甲酸二乙酯中的一种或两种。
更加具体的，所述2,2,6,6-四甲基-4-氨基哌啶与间苯二甲酸二烷基酯的摩尔比为2.4:1～3.3:1，优选为2.9:1。
在本发明的技术方案中，所述溶剂选自甲苯、甲醇或乙醇中的一种。具体的，2,2,6,6-四甲基-4-氨基哌啶与溶剂的质量比为1:7～1:10， 此时反应物的溶解和搅拌状态最好。
在本发明的技术方案中，具体的，所述催化剂选自三甲基铝、二乙基铝、三丙基铝、三丁基铝或三异丙基铝中的一种或几种，优选为三甲基铝。更加具体的，催化剂占反应物(2,2,6,6-四甲基-4-氨基哌啶、间苯二甲酸二烷基酯和溶剂)总质量的0.5～3％。
在本发明的技术方案中，步骤(2)所得滤液中除了含有溶剂外，还含有催化剂和过量的2,2,6,6-四甲基-4-氨基哌啶，故步骤(2)所得滤液可以作为下一次反应时步骤(1)的反应溶剂进行套用，即将步骤(2)所得滤液作为下一次步骤(1)中的溶剂进行重新利用。
具体的，当步骤(2)中的滤液套用时，2,2,6,6-四甲基-4-氨基哌啶与间苯二甲酸二烷基酯的摩尔比为2.0:1～2.3:1，优选为2.23:1。
本发明以2,2,6,6-四甲基-4-氨基哌啶和间苯二甲酸二烷基酯为原料，通过氨解反应得到N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺，避免了采用酰氯参与反应，无需NaOH中和，无需处理含氯废水，后期污水处理相对容易，相对环境友好；而且反应中产生的滤液可以套用，降低了工业化生产成本，综上，本发明的制备方法具有工艺简单、原料利用率高的优点，而且利用本发明的方法制备得到的N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺具有产品质量好、无氯离子残留的优点。
具体实施方式
以下实施例用于说明本发明，但不用来限制本发明的范围。
实施例1
本实施例为N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺的制备方法，具体包括以下步骤：
(1)将12g的2,2,6,6-四甲基-4-氨基哌啶(约0.076mol)溶于100g的甲苯中，加入3.5g的催化剂三甲基铝，充分搅拌1～5min将其完全溶解后，加入5g的间苯二甲酸二甲酯(约0.026mol)，反应温度上升至 50℃，反应24h，得混合液；
(2)将步骤(1)得到的混合液经冷却、过滤后分别得到滤液和固体物质，固体物质经水洗干燥后即得N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺(白色粉末)，收率为90％，熔点为272.5℃，含量99.65％(HPLC)。
上述用水进行洗涤，具体为：去离子水洗涤3～5次。
上述过滤干燥，具体为：80℃干燥12h。
实施例2
本实施例为N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺的制备方法，具体包括以下步骤：
(1)将12g的2,2,6,6-四甲基-4-氨基哌啶(约0.076mol)溶于100g的甲苯中，加入3.5g的催化剂三甲基铝，充分搅拌将其完全溶解，之后加入5g的间苯二甲酸二乙酯(约0.023mol)，反应温度上升至50℃，反应24h，得混合液；
(2)将步骤(1)得到的混合液经冷却、过滤后分别得到滤液和固体物质，固体物质经水洗干燥后即得N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺(白色粉末)，收率为85％，熔点为272.0℃，含量98.87％(HPLC)。
实施例3
本实施例为N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺的制备方法，具体包括以下步骤：
(1)将10g的2,2,6,6-四甲基-4-氨基哌啶(约0.064mol)溶于100g的甲苯中，加入0.6g的催化剂三甲基铝，充分搅拌1～5min将其完全溶解后，加入5g的间苯二甲酸二甲酯(约0.026mol)，反应温度上升至50℃，反应24h，得混合液；
(2)将步骤(1)得到的混合液经冷却、过滤后分别得到滤液和固体物质，固体物质经水洗干燥后即得N,N-二(2,2,6,6-四甲基-4-哌啶 基)-1,3-苯二甲酰胺(白色粉末)，收率为83％，熔点为271.9℃，含量98.65％(HPLC)。
实施例4
本实施例为N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺的制备方法，具体包括以下步骤：
(1)将12g(约0.076mol)的2,2,6,6-四甲基-4-氨基哌啶溶于100g的甲醇中，加入3.5g的催化剂三甲基铝，充分搅拌1～5min将其完全溶解后，加入5g的间苯二甲酸二甲酯(约0.026mol)，反应温度上升至70℃，反应24h，得混合液；
(2)将步骤(1)得到的混合液经冷却、过滤后分别得到滤液和固体物质，固体物质经水洗干燥后即得N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺(白色粉末)，收率为84％，熔点为271.8℃，含量98.70％(HPLC)。
实施例5
本实施例为N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺的制备方法，具体包括以下步骤：
(1)将9g的2,2,6,6-四甲基-4-氨基哌啶(约0.058mol)溶于100g的实施例1步骤(2)得到的滤液中，加入3.5g的催化剂三甲基铝，充分搅拌1～5min将其完全溶解后，加入5g的间苯二甲酸二甲酯(约0.026mol)，反应温度上升至50℃，反应24h，得混合液；
(2)将步骤(1)得到的混合液经冷却、过滤后分别得到滤液和固体物质，固体物质经水洗干燥后即得N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺(白色粉末)，收率为88％，熔点为271.9℃，含量98.97％(HPLC)。
实施例6
本实施例与实施例1的区别仅在于，步骤(1)中间苯二甲酸二甲酯的加入量不同，在本实施例中间苯二甲酸二甲酯的加入量为4.46g (约为0.023mol)。
最终N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺的收率为80％，熔点为272.2℃，含量98.87％(HPLC)。
实施例7
本实施例与实施例1的区别仅在于，步骤(1)中间苯二甲酸二甲酯的加入量不同，在本实施例中苯二甲酸二甲酯的加入量为6.15g(约为0.032mol)。
最终N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺的收率为82％，熔点为272.1℃，含量98.83％(HPLC)。
实施例8
本实施例与实施例5的区别仅在于，步骤(1)中间苯二甲酸二甲酯的加入量不同，在本实施例中苯二甲酸二甲酯的加入量为5.63g(约为0.029mol)。
最终N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺的收率为80％，熔点为272.2℃，含量98.68％(HPLC)。
实施例9
本实施例与实施例5的区别仅在于，步骤(1)中间苯二甲酸二甲酯的加入量不同，在本实施例中苯二甲酸二甲酯的加入量为4.82g(约0.025mol)。
最终N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺的收率为83％，熔点为271.9℃，含量98.76％(HPLC)。
对比例1
对比例1与实施例的区别仅在于，在对比例1中未添加催化剂，其余步骤相同，最终并未得到N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺。
对比例2
对比例2与实施例的区别仅在于，在对比例2中以氯化铵作为催化 剂，其余步骤相同，最终并未得到N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺。
虽然，上文中已经用一般性说明及具体实施方案对本发明作了详尽的描述，但在本发明基础上，可以对之作一些修改或改进，这对本领域技术人员而言是显而易见的。因此，在不偏离本发明精神的基础上所做的这些修改或改进，均属于本发明要求保护的范围。

Claims (9)

  1. 一种尼龙耐候助剂的制备方法，其特征在于，包括以下步骤：在溶剂中，以2,2,6,6-四甲基-4-氨基哌啶和间苯二甲酸二烷基酯为原料，在催化剂的催化下发生酯的氨解反应得到N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺。
  2. 根据权利要求1所述的尼龙耐候助剂的制备方法，其特征在于，包括以下步骤：
    (1)将2,2,6,6-四甲基-4-氨基哌啶溶于溶剂中，加入催化剂，充分搅拌，再加入间苯二甲酸二烷基酯，在40～80℃条件下反应得到混合液；
    (2)将步骤(1)得到的混合液经冷却、过滤后分别得到滤液和固体物质，固体物质经水洗干燥后即得N,N-二(2,2,6,6-四甲基-4-哌啶基)-1,3-苯二甲酰胺。
  3. 根据权利要求1或2所述的制备方法，其特征在于，所述间苯二甲酸二烷基酯选自间苯二甲酸二甲酯或间苯二甲酸二乙酯中的一种或两种。
  4. 根据权利要求1或2所述的制备方法，其特征在于，所述2,2,6,6-四甲基-4-氨基哌啶与间苯二甲酸二烷基酯的摩尔比为2.4:1～3.3:1，优选为2.9:1。
  5. 根据权利要求1或2所述的制备方法，其特征在于，所述溶剂选自甲苯、甲醇或乙醇中的一种。
  6. 根据权利要求1或2所述的制备方法，其特征在于，所述催化剂选自三甲基铝、二乙基铝、三丙基铝、三丁基铝或三异丙基铝中的一种或几种，优选为三甲基铝。
  7. 根据权利要求1或2所述的制备方法，其特征在于，所述催化剂占反应物总质量的0.5～3.0％。
  8. 根据权利要求2～7任一项所述的制备方法，其特征在于，将 步骤(2)所得滤液作为下一次反应时步骤(1)的溶剂。
  9. 根据权利要求8所述的制备方法，其特征在于，步骤(1)中2,2,6,6-四甲基-4-氨基哌啶与间苯二甲酸二烷基酯的摩尔比为2.0:1～2.3:1，优选为2.23:1。
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