阅读说明：本技术 一种γ型甘氨酸的制备方法及γ型甘氨酸 (Preparation method of gamma-type glycine and gamma-type glycine ) 是由 陈风华 薛荣荣 满诺 于 2020-06-09 设计创作，主要内容包括：本发明提供了一种γ型甘氨酸的制备方法及γ型甘氨酸,涉及工业原料的制备工艺技术领域。该制备方法包括如下步骤：将甘氨酸原料与催化剂混合形成混合物；以及采用球磨法对上述混合物进行球磨处理后得到γ型甘氨酸。本发明的制备方法能够直接将甘氨酸原料α型甘氨酸完全转变为γ型甘氨酸,制备过程中无需对生产过程进行调节,操作简单成熟。另外,本发明实施例的γ型甘氨酸的制备方法中催化剂无毒惰性,制备后无需对产物γ型甘氨酸做后续分离处理,使得制备工艺更加简单。(The invention provides a preparation method of gamma-type glycine and the gamma-type glycine, and relates to the technical field of preparation processes of industrial raw materials. The preparation method comprises the following steps: mixing a glycine starting material with a catalyst to form a mixture; and ball-milling the mixture by adopting a ball milling method to obtain the gamma-type glycine. The preparation method can directly convert the glycine raw material alpha-type glycine into gamma-type glycine completely, does not need to adjust the production process in the preparation process, and is simple and mature in operation. In addition, the catalyst in the preparation method of the gamma-type glycine provided by the embodiment of the invention is nontoxic and inert, and the subsequent separation treatment of the product gamma-type glycine is not needed after the preparation, so that the preparation process is simpler.)

1. The preparation method of gamma-type glycine is characterized by comprising the following steps:

mixing a glycine starting material with a catalyst to form a mixture; and

and performing ball milling treatment on the mixture by adopting a ball milling method to obtain the gamma-type glycine.

2. The preparation method according to claim 1, wherein the mass ratio of the glycine raw material to the catalyst in the mixture is as follows: 500: (1-500).

3. The method according to claim 2, wherein the mass percentage of the catalyst in the mixture is 0.2 wt%.

4. The method according to claim 1, wherein the catalyst is one or more stable inorganic salts.

5. The preparation method according to claim 4, wherein the catalyst is selected from one or more of potassium chloride, potassium bromide, potassium sulfate, dipotassium hydrogen phosphate, potassium dihydrogen phosphate, sodium chloride, sodium bromide or sodium sulfate.

6. The method according to claim 1, wherein the glycine starting material is an α -type glycine.

7. The method of claim 1, wherein the step of ball milling the mixture by ball milling further comprises: grinding aid ingredients are added, and the grinding aid ingredients are water or ethanol.

8. The preparation method according to claim 7, wherein the ball milling treatment time is 10min to 2 h.

9. The method according to claim 8, wherein the ball-milling treatment temperature is from room temperature to 60 ℃.

10. Gamma-glycine prepared by the process according to any one of claims 1 to 9.

Technical Field

The invention relates to the technical field of preparation processes of industrial raw materials, and particularly relates to a preparation method of gamma-type glycine and the gamma-type glycine.

Background

Glycine is an amino acid with the simplest structure, and is an important raw material in the fields of food, medicine and the like. The common glycine crystal forms are 3 types: alpha, beta and gamma forms. Where gamma-type is the stable phase, alpha-type is the metastable phase and beta-type is the unstable phase. The α form exists stably under low-temperature drying conditions, but the α form is transformed into the stable phase γ form under a moist heat environment. Due to crystallization kinetics problems, metastable-phase alpha-forms are generally preferentially obtained during the preparation of glycine crystals in aqueous solution. If crystal form transformation occurs in the process of storing and transporting the alpha-type glycine, the product is agglomerated, and the use is inconvenient. The gamma-type glycine is an advanced and excellent piezoelectric material and nonlinear optical material due to a special asymmetric polar structure. Therefore, the gamma-type glycine can effectively solve the problem of poor stability of glycine products and improve the using effect of the glycine products.

At present, the glycine products abroad are mainly gamma-type. The nucleation and growth of gamma-type glycine are very sensitive, the method for preparing gamma-type glycine is mainly a solution phase method, such as crystallization preparation in glycine solution which is treated by acidification and alkalization or added with alkali metal salt, and preparation by heating and converting alpha-type glycine in glycine aqueous solution with a specified pH value, but the preparation process and conditions are not easy to control, and the gamma-type glycine prepared by the solution phase needs to be obtained by separating a final product.

Disclosure of Invention

The invention aims to provide a preparation method of gamma-type glycine, which is cheap, simple and convenient to operate and does not need to be separated.

The invention also aims to provide gamma-type glycine.

The technical problem to be solved by the invention is realized by adopting the following technical scheme.

The invention provides a preparation method of gamma-type glycine, which is characterized by comprising the following steps:

mixing a glycine starting material with a catalyst to form a mixture; and

and performing ball milling treatment on the mixture by adopting a ball milling method to obtain the gamma-type glycine.

According to a preferred embodiment, the mass ratio of the glycine starting material to the catalyst in the mixture is: 500: (1-500).

According to a preferred embodiment, the mass percentage of catalyst in the mixture is 0.2 wt%.

According to a preferred embodiment, the catalyst is one or more of stabilized inorganic salts.

According to a preferred embodiment, the catalyst is selected from one or more of potassium chloride, potassium bromide, potassium sulfate, dipotassium hydrogen phosphate, potassium dihydrogen phosphate, sodium chloride, sodium bromide or sodium sulfate.

According to a preferred embodiment, the glycine starting material is an alpha-glycine.

According to a preferred embodiment, the step of ball milling the mixture by ball milling further comprises: grinding aid ingredients are added, and the grinding aid ingredients are water or ethanol.

According to a preferred embodiment, the ball milling treatment time is between 10min and 2 h.

According to a preferred embodiment, the ball milling treatment temperature is from ambient temperature to 60 ℃.

The invention also provides gamma-type glycine prepared by the preparation method.

Based on the technical scheme, the preparation method of the gamma-type glycine at least has the following technical effects:

the preparation method of the gamma-type glycine provided by the invention comprises the steps of mixing glycine raw materials and a catalyst to form a mixture, and then carrying out ball milling treatment on the mixture by adopting a ball milling method to obtain the gamma-type glycine. Under the combined action of physical ball milling and a catalyst, the preparation method can directly and completely convert the glycine raw material alpha-type glycine into gamma-type glycine, does not need to adjust the production process in the preparation process, and is simple and mature in operation.

In addition, the catalyst in the preparation method of the gamma-type glycine provided by the embodiment of the invention is nontoxic and inert, and the subsequent separation treatment of the product gamma-type glycine is not needed after the preparation, so that the preparation process is simpler.

Drawings

In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.

FIG. 1 is an XRD pattern of a product prepared according to example 1 of the present invention;

FIG. 2 is an XRD pattern of a product prepared according to example 2 of the present invention;

figure 3 is an XRD pattern of the product prepared in example 3 of the present invention.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.

The method for producing gamma-type glycine according to the embodiment of the present invention will be specifically described below.

The invention provides a preparation method of gamma-type glycine, which comprises the following steps:

mixing a glycine starting material with a catalyst to form a mixture; and

and performing ball milling treatment on the mixture by adopting a ball milling method to obtain the gamma-type glycine.

Preferably, the mass ratio of the glycine raw material to the catalyst in the mixture is as follows: 500: (1-500). Preferably, the mass percentage of catalyst in the mixture is 0.2 wt%. Preferably, the catalyst is one or more of stable inorganic salts. Preferably, the catalyst is selected from one or more of potassium chloride, potassium bromide, potassium sulfate, dipotassium hydrogen phosphate, potassium dihydrogen phosphate, sodium chloride, sodium bromide or sodium sulfate. Therefore, the catalyst content in the mixture can be very low, and the mixture is non-toxic and inert, so that the subsequent separation treatment of the prepared gamma-type glycine is not needed, and the treatment process is simplified.

Preferably, the glycine starting material is alpha-glycine.

Preferably, the step of ball milling the mixture by ball milling further comprises: grinding aid components are added, and grinding aid components are added into water or ethanol. Preferably, the ball milling treatment time is 10min-2 h. Preferably, the ball milling treatment temperature is from room temperature to 60 ℃. The preparation method is simple and mature, can directly and completely convert the alpha-type glycine raw material into the gamma-type glycine, and does not need to adjust the process in the preparation process.

The invention also provides gamma-type glycine prepared by the preparation method. The gamma-type glycine prepared by the preparation method has higher purity.

The features and properties of the present invention are described in further detail below with reference to examples.